Eco-analytical Methodology in Environmental Problems Monitoring

Science.gov (United States)

Agienko, M. I.; Bondareva, E. P.; Chistyakova, G. V.; Zhironkina, O. V.; Kalinina, O. I.

2017-01-01

Among the problems common to all mankind, which solutions influence the prospects of civilization, the problem of ecological situation monitoring takes very important place. Solution of this problem requires specific methodology based on eco-analytical comprehension of global issues. Eco-analytical methodology should help searching for the optimum balance between environmental problems and accelerating scientific and technical progress. The fact that Governments, corporations, scientists and nations focus on the production and consumption of material goods cause great damage to environment. As a result, the activity of environmentalists is developing quite spontaneously, as a complement to productive activities. Therefore, the challenge posed by the environmental problems for the science is the formation of geo-analytical reasoning and the monitoring of global problems common for the whole humanity. So it is expected to find the optimal trajectory of industrial development to prevent irreversible problems in the biosphere that could stop progress of civilization.

Determination of radium isotopes in environmental samples by gamma spectrometry, liquid scintillation counting and alpha spectrometry: a review of analytical methodology

International Nuclear Information System (INIS)

Jia, Guogang; Jia, Jing

2012-01-01

Radium (Ra) isotopes are important from the viewpoints of radiation protection and environmental protection. Their high toxicity has stimulated the continuing interest in methodology research for determination of Ra isotopes in various media. In this paper, the three most routinely used analytical techniques for Ra isotope determination in biological and environmental samples, i.e. low-background γ-spectrometry, liquid scintillation counting and α-spectrometry, were reviewed, with emphasis on new methodological developments in sample preparation, preconcentration, separation, purification, source preparation and measurement techniques. The accuracy, selectivity, traceability, applicability and minimum detectable activity (MDA) of the three techniques were discussed. It was concluded that the MDA (0.1 mBq L −1 ) of the α-spectrometry technique coupled with chemical separation is about two orders of magnitude lower than that of low-background HPGe γ-spectrometry and LSC techniques. Therefore, when maximum sensitivity is required, the α-spectrometry technique remains the first choice. - Highlights: ► A review is made for determination of Ra isotopes in environmental samples. ► Gamma spectrometry, LSC and a-spectrometry are the main concerned radiometric approach. ► Sample preparation, preconcentration, separation and source preparation are discussed. ► The methods can analyse air, water, seawater, soil, sediment and foodstuffs samples. ► Some new data obtained recently from our laboratory for Ra method study are included.

Validation of an analytical methodology for the quantitative analysis of petroleum hydrocarbons in marine sediment samples

Directory of Open Access Journals (Sweden)

Eloy Yordad Companioni Damas

2009-01-01

Full Text Available This work describes a validation of an analytical procedure for the analysis of petroleum hydrocarbons in marine sediment samples. The proposed protocol is able to measure n-alkanes and polycyclic aromatic hydrocarbons (PAH in samples at concentrations as low as 30 ng/g, with a precision better than 15% for most of analytes. The extraction efficiency of fortified sediments varied from 65.1 to 105.6% and 59.7 to 97.8%, for n-alkanes and PAH in the ranges: C16 - C32 and fluoranthene - benzo(apyrene, respectively. The analytical protocol was applied to determine petroleum hydrocarbons in sediments collected from a marine coastal zone.

A Big Data Analytics Methodology Program in the Health Sector

Science.gov (United States)

Lawler, James; Joseph, Anthony; Howell-Barber, H.

2016-01-01

The benefits of Big Data Analytics are cited frequently in the literature. However, the difficulties of implementing Big Data Analytics can limit the number of organizational projects. In this study, the authors evaluate business, procedural and technical factors in the implementation of Big Data Analytics, applying a methodology program. Focusing…

Analytical Chemistry as Methodology in Modern Pure and Applied Chemistry

OpenAIRE

Honjo, Takaharu

2001-01-01

Analytical chemistry is an indispensable methodology in pure and applied chemistry, which is often compared to a foundation stone of architecture. In the home page of jsac, it is said that analytical chemistry is a learning of basic science, which treats the development of method in order to get usefull chemical information of materials by means of detection, separation, and characterization. Analytical chemistry has recently developed into analytical sciences, which treats not only analysis ...

Sample size methodology

CERN Document Server

Desu, M M

2012-01-01

One of the most important problems in designing an experiment or a survey is sample size determination and this book presents the currently available methodology. It includes both random sampling from standard probability distributions and from finite populations. Also discussed is sample size determination for estimating parameters in a Bayesian setting by considering the posterior distribution of the parameter and specifying the necessary requirements. The determination of the sample size is considered for ranking and selection problems as well as for the design of clinical trials. Appropria

A rapid and sensitive analytical method for the determination of 14 pyrethroids in water samples.

Science.gov (United States)

Feo, M L; Eljarrat, E; Barceló, D

2010-04-09

A simple, efficient and environmentally friendly analytical methodology is proposed for extracting and preconcentrating pyrethroids from water samples prior to gas chromatography-negative ion chemical ionization mass spectrometry (GC-NCI-MS) analysis. Fourteen pyrethroids were selected for this work: bifenthrin, cyfluthrin, lambda-cyhalothrin, cypermethrin, deltamethrin, esfenvalerate, fenvalerate, fenpropathrin, tau-fluvalinate, permethrin, phenothrin, resmethrin, tetramethrin and tralomethrin. The method is based on ultrasound-assisted emulsification-extraction (UAEE) of a water-immiscible solvent in an aqueous medium. Chloroform was used as extraction solvent in the UAEE technique. Target analytes were quantitatively extracted achieving an enrichment factor of 200 when 20 mL aliquot of pure water spiked with pyrethroid standards was extracted. The method was also evaluated with tap water and river water samples. Method detection limits (MDLs) ranged from 0.03 to 35.8 ng L(-1) with RSDs values or =0.998. Recovery values were in the range of 45-106%, showing satisfactory robustness of the method for analyzing pyrethroids in water samples. The proposed methodology was applied for the analysis of river water samples. Cypermethrin was detected at concentration levels ranging from 4.94 to 30.5 ng L(-1). Copyright 2010 Elsevier B.V. All rights reserved.

Developing Foucault's Discourse Analytic Methodology

Directory of Open Access Journals (Sweden)

Rainer Diaz-Bone

2006-01-01

Full Text Available A methodological position for a FOUCAULTian discourse analysis is presented. A sequence of analytical steps is introduced and an illustrating example is offered. It is emphasized that discourse analysis has to discover the system-level of discursive rules and the deeper structure of the discursive formation. Otherwise the analysis will be unfinished. Michel FOUCAULTs work is theoretically grounded in French structuralism and (the so called post-structuralism. In this paper, post-structuralism is not conceived as a means for overcoming of structuralism, but as a way of critically continuing the structural perspective. In this way, discursive structures can be related to discursive practices and the concept of structure can be disclosed (e. g. to inter-discourse or DERRIDAs concept of structurality. In this way, the structural methodology is continued and radicalized, but not given up. In this paper, FOUCAULTs theory is combined with the works of Michel PÊCHEUX and (especially for the sociology of knowledge and the sociology of culture Pierre BOURDIEU. The practice of discourse analysis is theoretically grounded. This practice can be conceived as a reflexive coupling of deconstruction and reconstruction in the material to be analyzed. This methodology therefore can be characterized as a reconstructive qualitative methodology. At the end of the article, forms of discourse analysis are criticized that do not intend to recover the system level of discursive rules and that do not intend to discover the deeper structure of the discursive formation (i. e. episteme, socio-episteme. These forms merely are commentaries of discourses (not their analyses, they remain phenomenological and are therefore: pre-structuralist. URN: urn:nbn:de:0114-fqs060168

Distinguishing between satisfaction and loyalty: Conceptual, methodological & analytical differences

Energy Technology Data Exchange (ETDEWEB)

Hinson, K.A. [Illinois Power, Decatur, IL (United States)

1994-11-01

This paper briefly presents a discussion of the conceptual definition of {open_quotes}Customer Satisfaction{close_quotes} followed by review of operational definitions of {open_quotes}Satisfaction{close_quotes} as a criterion variable and the kinds of predictor variables and analytic methods employed in its modeling. A model of {open_quotes}Customer Satisfaction{close_quotes} is presented developed by the discussed methodology. Conceptual and operational definitions of {open_quotes}Customer Loyalty{close_quotes} are then reviewed, contrasting the kinds of predictor variables and analytic methods most appropriate for understanding a {open_quotes}Loyalty{close_quotes} decision and how these differ from {open_quotes}Customer Satisfaction.{close_quotes} A more fully specified model of {open_quotes}Customer Loyalty{close_quotes} is presented. Finally, the risks of employing a {open_quotes}Satisfaction{close_quotes} methodology in modeling {open_quotes}Customer Loyalty{close_quotes} are discussed.

MS-based analytical methodologies to characterize genetically modified crops.

Science.gov (United States)

García-Cañas, Virginia; Simó, Carolina; León, Carlos; Ibáñez, Elena; Cifuentes, Alejandro

2011-01-01

The development of genetically modified crops has had a great impact on the agriculture and food industries. However, the development of any genetically modified organism (GMO) requires the application of analytical procedures to confirm the equivalence of the GMO compared to its isogenic non-transgenic counterpart. Moreover, the use of GMOs in foods and agriculture faces numerous criticisms from consumers and ecological organizations that have led some countries to regulate their production, growth, and commercialization. These regulations have brought about the need of new and more powerful analytical methods to face the complexity of this topic. In this regard, MS-based technologies are increasingly used for GMOs analysis to provide very useful information on GMO composition (e.g., metabolites, proteins). This review focuses on the MS-based analytical methodologies used to characterize genetically modified crops (also called transgenic crops). First, an overview on genetically modified crops development is provided, together with the main difficulties of their analysis. Next, the different MS-based analytical approaches applied to characterize GM crops are critically discussed, and include "-omics" approaches and target-based approaches. These methodologies allow the study of intended and unintended effects that result from the genetic transformation. This information is considered to be essential to corroborate (or not) the equivalence of the GM crop with its isogenic non-transgenic counterpart. Copyright © 2010 Wiley Periodicals, Inc.

Post-analytical stability of 23 common chemistry and immunochemistry analytes in incurred samples

DEFF Research Database (Denmark)

Nielsen, Betina Klint; Frederiksen, Tina; Friis-Hansen, Lennart

2017-01-01

BACKGROUND: Storage of blood samples after centrifugation, decapping and initial sampling allows ordering of additional blood tests. The pre-analytic stability of biochemistry and immunochemistry analytes has been studied in detail, but little is known about the post-analytical stability...... in incurred samples. METHODS: We examined the stability of 23 routine analytes on the Dimension Vista® (Siemens Healthineers, Denmark): 42-60 routine samples in lithium-heparin gel tubes (Vacutainer, BD, USA) were centrifuged at 3000×g for 10min. Immediately after centrifugation, initial concentration...... of analytes were measured in duplicate (t=0). The tubes were stored decapped at room temperature and re-analyzed after 2, 4, 6, 8 and 10h in singletons. The concentration from reanalysis were normalized to initial concentration (t=0). Internal acceptance criteria for bias and total error were used...

Developing a business analytics methodology: a case study in the foodbank sector

OpenAIRE

Hindle, Giles; Vidgen, Richard

2017-01-01

The current research seeks to address the following question: how can organizations align their business analytics development projects with their business goals? To pursue this research agenda we adopt an action research framework to develop and apply a business analytics methodology (BAM). The four-stage BAM (problem situation structuring, business model mapping, analytics leverage analysis, and analytics implementation) is not a prescription. Rather, it provides a logical structure and log...

Transuranium analysis methodologies for biological and environmental samples

International Nuclear Information System (INIS)

Wessman, R.A.; Lee, K.D.; Curry, B.; Leventhal, L.

1978-01-01

Analytical procedures for the most abundant transuranium nuclides in the environment (i.e., plutonium and, to a lesser extent, americium) are available. There is a lack of procedures for doing sequential analysis for Np, Pu, Am, and Cm in environmental samples, primarily because of current emphasis on Pu and Am. Reprocessing requirements and waste disposal connected with the fuel cycle indicate that neptunium and curium must be considered in environmental radioactive assessments. Therefore it was necessary to develop procedures that determine all four of these radionuclides in the environment. The state of the art of transuranium analysis methodology as applied to environmental samples is discussed relative to different sample sources, such as soil, vegetation, air, water, and animals. Isotope-dilution analysis with 243 Am ( 239 Np) and 236 Pu or 242 Pu radionuclide tracers is used. Americium and curium are analyzed as a group, with 243 Am as the tracer. Sequential extraction procedures employing bis(2-ethyl-hexyl)orthophosphoric acid (HDEHP) were found to result in lower yields and higher Am--Cm fractionation than ion-exchange methods

Field screening sampling and analysis strategy and methodology for the 183-H Solar Evaporation Basins: Phase 2, Soils

International Nuclear Information System (INIS)

Antipas, A.; Hopkins, A.M.; Wasemiller, M.A.; McCain, R.G.

1996-01-01

This document provides a sampling/analytical strategy and methodology for Resource Conservation and Recovery Act (RCRA) closure of the 183-H Solar Evaporation Basins within the boundaries and requirements identified in the initial Phase II Sampling and Analysis Plan for RCRA Closure of the 183-H Solar Evaporation Basins

Bias Assessment of General Chemistry Analytes using Commutable Samples.

Science.gov (United States)

Koerbin, Gus; Tate, Jillian R; Ryan, Julie; Jones, Graham Rd; Sikaris, Ken A; Kanowski, David; Reed, Maxine; Gill, Janice; Koumantakis, George; Yen, Tina; St John, Andrew; Hickman, Peter E; Simpson, Aaron; Graham, Peter

2014-11-01

Harmonisation of reference intervals for routine general chemistry analytes has been a goal for many years. Analytical bias may prevent this harmonisation. To determine if analytical bias is present when comparing methods, the use of commutable samples, or samples that have the same properties as the clinical samples routinely analysed, should be used as reference samples to eliminate the possibility of matrix effect. The use of commutable samples has improved the identification of unacceptable analytical performance in the Netherlands and Spain. The International Federation of Clinical Chemistry and Laboratory Medicine (IFCC) has undertaken a pilot study using commutable samples in an attempt to determine not only country specific reference intervals but to make them comparable between countries. Australia and New Zealand, through the Australasian Association of Clinical Biochemists (AACB), have also undertaken an assessment of analytical bias using commutable samples and determined that of the 27 general chemistry analytes studied, 19 showed sufficiently small between method biases as to not prevent harmonisation of reference intervals. Application of evidence based approaches including the determination of analytical bias using commutable material is necessary when seeking to harmonise reference intervals.

Hanford analytical sample projections FY 1998 - FY 2002

International Nuclear Information System (INIS)

Joyce, S.M.

1998-01-01

Analytical Services projections are compiled for the Hanford site based on inputs from the major programs for the years 1998 through 2002. Projections are categorized by radiation level, protocol, sample matrix and program. Analyses requirements are also presented. This document summarizes the Hanford sample projections for fiscal years 1998 to 2002. Sample projections are based on inputs submitted to Analytical Services covering Environmental Restoration, Tank Waste Remediation Systems (TWRS), Solid Waste, Liquid Effluents, Spent Nuclear Fuels, Transition Projects, Site Monitoring, Industrial Hygiene, Analytical Services and miscellaneous Hanford support activities. In addition, details on laboratory scale technology (development) work, Sample Management, and Data Management activities are included. This information will be used by Hanford Analytical Services (HAS) and the Sample Management Working Group (SMWG) to assure that laboratories and resources are available and effectively utilized to meet these documented needs

Hanford analytical sample projections FY 1998--FY 2002

Energy Technology Data Exchange (ETDEWEB)

Joyce, S.M.

1998-02-12

Analytical Services projections are compiled for the Hanford site based on inputs from the major programs for the years 1998 through 2002. Projections are categorized by radiation level, protocol, sample matrix and program. Analyses requirements are also presented. This document summarizes the Hanford sample projections for fiscal years 1998 to 2002. Sample projections are based on inputs submitted to Analytical Services covering Environmental Restoration, Tank Waste Remediation Systems (TWRS), Solid Waste, Liquid Effluents, Spent Nuclear Fuels, Transition Projects, Site Monitoring, Industrial Hygiene, Analytical Services and miscellaneous Hanford support activities. In addition, details on laboratory scale technology (development) work, Sample Management, and Data Management activities are included. This information will be used by Hanford Analytical Services (HAS) and the Sample Management Working Group (SMWG) to assure that laboratories and resources are available and effectively utilized to meet these documented needs.

Sampling methodology and PCB analysis

International Nuclear Information System (INIS)

Dominelli, N.

1995-01-01

As a class of compounds PCBs are extremely stable and resist chemical and biological decomposition. Diluted solutions exposed to a range of environmental conditions will undergo some preferential degradation and the resulting mixture may differ considerably from the original PCB used as insulating fluid in electrical equipment. The structure of mixtures of PCBs (synthetic compounds prepared by direct chlorination of biphenyl with chlorine gas) is extremely complex and presents a formidable analytical problem, further complicated by the presence of PCBs as contaminants in oils to soils to water. This paper provides some guidance into sampling and analytical procedures; it also points out various potential problems encountered during these processes. The guidelines provided deal with sample collection, storage and handling, sample stability, laboratory analysis (usually gas chromatography), determination of PCB concentration, calculation of total PCB content, and quality assurance. 1 fig

Towards Standardization of Sampling Methodology for Evaluation of ...

African Journals Online (AJOL)

This article proposes the procedure that may be adopted for comparable, representative and cost effective, soil sampling, and thereafter explores the policy issues regarding standardization of sampling activities and analytical process as it relates to soil pollution in Nigeria. Standardized sampling and analytical data for soil ...

Marine anthropogenic radiotracers in the Southern Hemisphere: New sampling and analytical strategies

Science.gov (United States)

Levy, I.; Povinec, P. P.; Aoyama, M.; Hirose, K.; Sanchez-Cabeza, J. A.; Comanducci, J.-F.; Gastaud, J.; Eriksson, M.; Hamajima, Y.; Kim, C. S.; Komura, K.; Osvath, I.; Roos, P.; Yim, S. A.

2011-04-01

The Japan Agency for Marine Earth Science and Technology conducted in 2003-2004 the Blue Earth Global Expedition (BEAGLE2003) around the Southern Hemisphere Oceans, which was a rare opportunity to collect many seawater samples for anthropogenic radionuclide studies. We describe here sampling and analytical methodologies based on radiochemical separations of Cs and Pu from seawater, as well as radiometric and mass spectrometry measurements. Several laboratories took part in radionuclide analyses using different techniques. The intercomparison exercises and analyses of certified reference materials showed a reasonable agreement between the participating laboratories. The obtained data on the distribution of 137Cs and plutonium isotopes in seawater represent the most comprehensive results available for the Southern Hemisphere Oceans.

A new tool for the evaluation of the analytical procedure: Green Analytical Procedure Index.

Science.gov (United States)

Płotka-Wasylka, J

2018-05-01

A new means for assessing analytical protocols relating to green analytical chemistry attributes has been developed. The new tool, called GAPI (Green Analytical Procedure Index), evaluates the green character of an entire analytical methodology, from sample collection to final determination, and was created using such tools as the National Environmental Methods Index (NEMI) or Analytical Eco-Scale to provide not only general but also qualitative information. In GAPI, a specific symbol with five pentagrams can be used to evaluate and quantify the environmental impact involved in each step of an analytical methodology, mainly from green through yellow to red depicting low, medium to high impact, respectively. The proposed tool was used to evaluate analytical procedures applied in the determination of biogenic amines in wine samples, and polycyclic aromatic hydrocarbon determination by EPA methods. GAPI tool not only provides an immediately perceptible perspective to the user/reader but also offers exhaustive information on evaluated procedures. Copyright © 2018 Elsevier B.V. All rights reserved.

Sampling Large Graphs for Anticipatory Analytics

Science.gov (United States)

2015-05-15

low. C. Random Area Sampling Random area sampling [8] is a “ snowball ” sampling method in which a set of random seed vertices are selected and areas... Sampling Large Graphs for Anticipatory Analytics Lauren Edwards, Luke Johnson, Maja Milosavljevic, Vijay Gadepally, Benjamin A. Miller Lincoln...systems, greater human-in-the-loop involvement, or through complex algorithms. We are investigating the use of sampling to mitigate these challenges

Sampling analytical tests and destructive tests for quality assurance

International Nuclear Information System (INIS)

Saas, A.; Pasquini, S.; Jouan, A.; Angelis, de; Hreen Taywood, H.; Odoj, R.

1990-01-01

In the context of the third programme of the European Communities on the monitoring of radioactive waste, various methods have been developed for the performance of sampling and measuring tests on encapsulated waste of low and medium level activity, on the one hand, and of high level activity, on the other hand. The purpose was to provide better quality assurance for products to be stored on an interim or long-term basis. Various testing sampling means are proposed such as: - sampling of raw waste before conditioning and determination of the representative aliquot, - sampling of encapsulated waste on process output, - sampling of core specimens subjected to measurement before and after cutting. Equipment suitable for these sampling procedures have been developed and, in the case of core samples, a comparison of techniques has been made. The results are described for the various analytical tests carried out on the samples such as: - mechanical tests, - radiation resistance, - fire resistance, - lixiviation, - determination of free water, - biodegradation, - water resistance, - chemical and radiochemical analysis. Every time it was possible, these tests were compared with non-destructive tests on full-scale packages and some correlations are given. This word has made if possible to improve and clarify sample optimization, with fine sampling techniques and methodologies and draw up characterization procedures. It also provided an occasion for a first collaboration between the laboratories responsible for these studies and which will be furthered in the scope of the 1990-1994 programme

Analytical Chemistry Division's sample transaction system

International Nuclear Information System (INIS)

Stanton, J.S.; Tilson, P.A.

1980-10-01

The Analytical Chemistry Division uses the DECsystem-10 computer for a wide range of tasks: sample management, timekeeping, quality assurance, and data calculation. This document describes the features and operating characteristics of many of the computer programs used by the Division. The descriptions are divided into chapters which cover all of the information about one aspect of the Analytical Chemistry Division's computer processing

Registration-analytical maintenance and methodological features of construction of the financial account

OpenAIRE

Kraevskyy, V.

2009-01-01

In article registration-analytical maintenance and methodological features of construction of the financial account is considered. Financial account, net lending, net borrowing, financial assets, system of the national accounts.

Methodology for sample preparation and size measurement of commercial ZnO nanoparticles

Directory of Open Access Journals (Sweden)

Pei-Jia Lu

2018-04-01

Full Text Available This study discusses the strategies on sample preparation to acquire images with sufficient quality for size characterization by scanning electron microscope (SEM using two commercial ZnO nanoparticles of different surface properties as a demonstration. The central idea is that micrometer sized aggregates of ZnO in powdered forms need to firstly be broken down to nanosized particles through an appropriate process to generate nanoparticle dispersion before being deposited on a flat surface for SEM observation. Analytical tools such as contact angle, dynamic light scattering and zeta potential have been utilized to optimize the procedure for sample preparation and to check the quality of the results. Meanwhile, measurements of zeta potential values on flat surfaces also provide critical information and save lots of time and efforts in selection of suitable substrate for particles of different properties to be attracted and kept on the surface without further aggregation. This simple, low-cost methodology can be generally applied on size characterization of commercial ZnO nanoparticles with limited information from vendors. Keywords: Zinc oxide, Nanoparticles, Methodology

A Model-Driven Methodology for Big Data Analytics-as-a-Service

OpenAIRE

Damiani, Ernesto; Ardagna, Claudio Agostino; Ceravolo, Paolo; Bellandi, Valerio; Bezzi, Michele; Hebert, Cedric

2017-01-01

The Big Data revolution has promised to build a data-driven ecosystem where better decisions are supported by enhanced analytics and data management. However, critical issues still need to be solved in the road that leads to commodization of Big Data Analytics, such as the management of Big Data complexity and the protection of data security and privacy. In this paper, we focus on the first issue and propose a methodology based on Model Driven Engineering (MDE) that aims to substantially lowe...

Soviet-designed pressurized water reactor symptomatic emergency operating instruction analytical procedure: approach, methodology, development and application

International Nuclear Information System (INIS)

Beelman, R.J.

1999-01-01

A symptom approach to the analytical validation of symptom-based EOPs includes: (1) Identification of critical safety functions to the maintenance of fission product barrier integrity; (2) Identification of the symptoms which manifest an impending challenge to critical safety function maintenance; (3) Development of a symptomatic methodology to delineate bounding plant transient response modes; (4) Specification of bounding scenarios; (5) Development of a systematic calculational approach consistent with the objectives of the methodology; (6) Performance of thermal-hydraulic computer code calculations implementing the analytical methodology; (7) Interpretation of the analytical results on the basis of information available to the operator; (8) Application of the results to the validation of the proposed operator actions; (9) Production of a technical basis document justifying the proposed operator actions. (author)

Paper-Based Analytical Device for Zinc Ion Quantification in Water Samples with Power-Free Analyte Concentration

Directory of Open Access Journals (Sweden)

Hiroko Kudo

2017-04-01

Full Text Available Insufficient sensitivity is a general issue of colorimetric paper-based analytical devices (PADs for trace analyte detection, such as metal ions, in environmental water. This paper demonstrates the colorimetric detection of zinc ions (Zn2+ on a paper-based analytical device with an integrated analyte concentration system. Concentration of Zn2+ ions from an enlarged sample volume (1 mL has been achieved with the aid of a colorimetric Zn2+ indicator (Zincon electrostatically immobilized onto a filter paper substrate in combination with highly water-absorbent materials. Analyte concentration as well as sample pretreatment, including pH adjustment and interferent masking, has been elaborated. The resulting device enables colorimetric quantification of Zn2+ in environmental water samples (tap water, river water from a single sample application. The achieved detection limit of 0.53 μM is a significant improvement over that of a commercial colorimetric Zn2+ test paper (9.7 μM, demonstrating the efficiency of the developed analyte concentration system not requiring any equipment.

D4.1 Learning analytics: theoretical background, methodology and expected results

NARCIS (Netherlands)

Tammets, Kairit; Laanpere, Mart; Eradze, Maka; Brouns, Francis; Padrón-Nápoles, Carmen; De Rosa, Rosanna; Ferrari, Chiara

2014-01-01

The purpose of the EMMA project is to showcase excellence in innovative teaching methodologies and learning approaches through the large-scale piloting of MOOCs on different subjects. The main objectives related with the implementation of learning analytics in EMMa project are to: ● develop the

Development of analytical techniques for safeguards environmental samples at JAEA

International Nuclear Information System (INIS)

Sakurai, Satoshi; Magara, Masaaki; Usuda, Shigekazu; Watanabe, Kazuo; Esaka, Fumitaka; Hirayama, Fumio; Lee, Chi-Gyu; Yasuda, Kenichiro; Inagawa, Jun; Suzuki, Daisuke; Iguchi, Kazunari; Kokubu, Yoko S.; Miyamoto, Yutaka; Ohzu, Akira

2007-01-01

JAEA has been developing, under the auspices of the Ministry of Education, Culture, Sports, Science and Technology of Japan, analytical techniques for ultra-trace amounts of nuclear materials in environmental samples in order to contribute to the strengthened safeguards system. Development of essential techniques for bulk and particle analysis, as well as screening, of the environmental swipe samples has been established as ultra-trace analytical methods of uranium and plutonium. In January 2003, JAEA was qualified, including its quality control system, as a member of the JAEA network analytical laboratories for environmental samples. Since 2004, JAEA has conducted the analysis of domestic and the IAEA samples, through which JAEA's analytical capability has been verified and improved. In parallel, advanced techniques have been developed in order to expand the applicability to the samples of various elemental composition and impurities and to improve analytical accuracy and efficiency. This paper summarizes the trace of the technical development in environmental sample analysis at JAEA, and refers to recent trends of research and development in this field. (author)

Analytical methodology and facility description spent fuel policy

Energy Technology Data Exchange (ETDEWEB)

1978-08-01

Three generic environmental impact statements (GEISs) on domestic fuels, foreign fuels, and storage charges are being prepared to provide environmental input into decisions on whether, and if so how the 1977 Presidential policy on spent fuel storage should be implmented. This report provides background information for two of these environmental impact statements: Storage of U.S. Spent Power Reactor Fuel and Storage of Foreign Spent Power Reactor Fuel. It includes the analytical methodology used in GEISs to assess the environmental effects and a description of the facilities used in the two GEISs.

Analytical methodology and facility description spent fuel policy

International Nuclear Information System (INIS)

1978-08-01

Three generic environmental impact statements (GEISs) on domestic fuels, foreign fuels, and storage charges are being prepared to provide environmental input into decisions on whether, and if so how the 1977 Presidential policy on spent fuel storage should be implmented. This report provides background information for two of these environmental impact statements: Storage of U.S. Spent Power Reactor Fuel and Storage of Foreign Spent Power Reactor Fuel. It includes the analytical methodology used in GEISs to assess the environmental effects and a description of the facilities used in the two GEISs

40 CFR 141.22 - Turbidity sampling and analytical requirements.

Science.gov (United States)

2010-07-01

... 40 Protection of Environment 22 2010-07-01 2010-07-01 false Turbidity sampling and analytical... § 141.22 Turbidity sampling and analytical requirements. The requirements in this section apply to... the water distribution system at least once per day, for the purposes of making turbidity measurements...

The analytical calibration in (bio)imaging/mapping of the metallic elements in biological samples--definitions, nomenclature and strategies: state of the art.

Science.gov (United States)

Jurowski, Kamil; Buszewski, Bogusław; Piekoszewski, Wojciech

2015-01-01

Nowadays, studies related to the distribution of metallic elements in biological samples are one of the most important issues. There are many articles dedicated to specific analytical atomic spectrometry techniques used for mapping/(bio)imaging the metallic elements in various kinds of biological samples. However, in such literature, there is a lack of articles dedicated to reviewing calibration strategies, and their problems, nomenclature, definitions, ways and methods used to obtain quantitative distribution maps. The aim of this article was to characterize the analytical calibration in the (bio)imaging/mapping of the metallic elements in biological samples including (1) nomenclature; (2) definitions, and (3) selected and sophisticated, examples of calibration strategies with analytical calibration procedures applied in the different analytical methods currently used to study an element's distribution in biological samples/materials such as LA ICP-MS, SIMS, EDS, XRF and others. The main emphasis was placed on the procedures and methodology of the analytical calibration strategy. Additionally, the aim of this work is to systematize the nomenclature for the calibration terms: analytical calibration, analytical calibration method, analytical calibration procedure and analytical calibration strategy. The authors also want to popularize the division of calibration methods that are different than those hitherto used. This article is the first work in literature that refers to and emphasizes many different and complex aspects of analytical calibration problems in studies related to (bio)imaging/mapping metallic elements in different kinds of biological samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Study of New Analytical Methodologies for the Analysis of Polychlorinated Dibenzo-P-Dioxins (PcDDs) and Polychlorinated Di benzofurans (PCDFs) by Quadrupole Ion Storage Tandem-in-time Mass Spectrometry. Application to Environmental Samples

International Nuclear Information System (INIS)

Sanz Chichon, M. P.

2008-01-01

Two alternative analytical methodologies have been developed for the analysis of polychlorinated dibenzo-p-dioxins ( PCDDs) and di benzofurans (PCDFs) in environmental samples. The techniques studied have been: Pressurized Fluid Extraction (PFE) and Microwave-Assisted Extraction (MAE) versus Soxhlet extraction; the automated system Power-PrepTM versus the conventional cleanup using open chromatographic columns with different adsorbents and the application of tandem mass spectrometry (HRGC-MS/MS) versus high resolution mass spectrometry (HRGC-HRMS) for PCDD/Fs detection and quantification. (Author) 233 refs

Hanford analytical sample projections FY 1996 - FY 2001. Revision 4

Energy Technology Data Exchange (ETDEWEB)

Joyce, S.M.

1997-07-02

This document summarizes the biannual Hanford sample projections for fiscal year 1997-2001. Sample projections are based on inputs submitted to Analytical Services covering Environmental Restoration, Tank Wastes Remediation Systems, Solid Wastes, Liquid Effluents, Spent Nuclear Fuels, Transition Projects, Site Monitoring, Industrial Hygiene, Analytical Services and miscellaneous Hanford support activities. In addition to this revision, details on Laboratory scale technology (development), Sample management, and Data management activities were requested. This information will be used by the Hanford Analytical Services program and the Sample Management Working Group to assure that laboratories and resources are available and effectively utilized to meet these documented needs.

Analytical methodology for the study of decontamination factors in mixer-settlers

International Nuclear Information System (INIS)

Alzabet, Horacio; Crubellati, Ricardo; Di Santo, Norberto; Eppis, Maria; Gonzalez, Guillermo; Bof, Elba; Devida, Claudio

1987-01-01

Due to the complexity of the samples, the choice of the analytical methodology to be applied at a radiochemical laboratory, for the evaluation of different separation steps if of a great importance. It is necessary to know the performance of mixer-settlers in two extreme situations: efficiency limit determined by fluid dynamic factors and separation factor determined by physicochemical variables. The element used to determine the efficiency limit was magnesium, due to its low distribution coefficient in tri-n-butyl phosphate (TBP). Zirconium, being one of the principal fission product, is partially extracted and was used to study the influence of chemical conditions. Atomic absorption spectrometry was selected for the determination of micro quantities of magnesium, and complexometry for macro quantities of this element. It was necessary to separate uranium using extraction chromatography with Kel F-TBP columns. Concentration range was 0.1 - 1 mg/L and 7 - 70 g/L respectively. Zirconium was determined by spectrophotometry with xylenol orange. For organic samples, it was necessary to reextract the analyte with fluoride, to evaporate with sulfuric acid and to complex the excess of fluoride with aluminum. Uranium determinations, required for mass balance, were carried out by spectrophotometry and potentiometry depending upon concentration. Because of the presence of zirconium, two methods were developed for uranium determination using liquid-liquid extraction in the presence of complexing agents. In one case, TBP was used as extractant, dibenzoylmethane as chromogenic reagent and EDTA as complexing agent. For very low quantities of uranium, tri-octyl phosphine oxide (TOPO) was the extractant, 2-(2-thiazolylazo)-5-diethylaminophenol (TAAP) the chromogenic reagent, and (1-2-cyclohexylenedinitrilo) tetraacetic acid (CDTA) the complexing agent. (Author)

Toward decentralized analysis of mercury (II) in real samples. A critical review on nanotechnology-based methodologies.

Science.gov (United States)

Botasini, Santiago; Heijo, Gonzalo; Méndez, Eduardo

2013-10-24

In recent years, it has increased the number of works focused on the development of novel nanoparticle-based sensors for mercury detection, mainly motivated by the need of low cost portable devices capable of giving fast and reliable analytical response, thus contributing to the analytical decentralization. Methodologies employing colorimetric, fluorometric, magnetic, and electrochemical output signals allowed reaching detection limits within the pM and nM ranges. Most of these developments proved their suitability in detecting and quantifying mercury (II) ions in synthetic solutions or spiked water samples. However, the state of art in these technologies is still behind the standard methods of mercury quantification, such as cold vapor atomic absorption spectrometry and inductively coupled plasma techniques, in terms of reliability and sensitivity. This is mainly because the response of nanoparticle-based sensors is highly affected by the sample matrix. The developed analytical nanosystems may fail in real samples because of the negative incidence of the ionic strength and the presence of exchangeable ligands. The aim of this review is to critically consider the recently published innovations in this area, and highlight the needs to include more realistic assays in future research in order to make these advances suitable for on-site analysis. Copyright © 2013 Elsevier B.V. All rights reserved.

New methodology for analytical calculation of resonance integrals in an heterogeneous medium

International Nuclear Information System (INIS)

Campos, T.P.R. de; Martinez, A.S.

1986-01-01

A new methodology for analytical calculation of Resonance Integral in a typical fuel cell is presented. The expression obtained for the Resonance Integral presents the advantage of being analytical. Its constituent terms are combinations of the well known function J(xi,β) with its partial derivatives in regard to β. This is a general expression for all types of resonance. The parameters used in this method depend on the resonance type and are obtained as a function of the parameter lambda. A simple expression, depending on resonance parameters is proposed for this variable. (Author) [pt

Contemporary sample stacking in analytical electrophoresis

Czech Academy of Sciences Publication Activity Database

Šlampová, Andrea; Malá, Zdeňka; Pantůčková, Pavla; Gebauer, Petr; Boček, Petr

2013-01-01

Roč. 34, č. 1 (2013), s. 3-18 ISSN 0173-0835 R&D Projects: GA ČR GAP206/10/1219 Institutional support: RVO:68081715 Keywords : biological samples * stacking * trace analysis * zone electrophoresis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.161, year: 2013

Contemporary sample stacking in analytical electrophoresis

Czech Academy of Sciences Publication Activity Database

Malá, Zdeňka; Šlampová, Andrea; Křivánková, Ludmila; Gebauer, Petr; Boček, Petr

2015-01-01

Roč. 36, č. 1 (2015), s. 15-35 ISSN 0173-0835 R&D Projects: GA ČR(CZ) GA13-05762S Institutional support: RVO:68081715 Keywords : biological samples * stacking * trace analysis * zone electrophoresis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.482, year: 2015

[Progress in sample preparation and analytical methods for trace polar small molecules in complex samples].

Science.gov (United States)

Zhang, Qianchun; Luo, Xialin; Li, Gongke; Xiao, Xiaohua

2015-09-01

Small polar molecules such as nucleosides, amines, amino acids are important analytes in biological, food, environmental, and other fields. It is necessary to develop efficient sample preparation and sensitive analytical methods for rapid analysis of these polar small molecules in complex matrices. Some typical materials in sample preparation, including silica, polymer, carbon, boric acid and so on, are introduced in this paper. Meanwhile, the applications and developments of analytical methods of polar small molecules, such as reversed-phase liquid chromatography, hydrophilic interaction chromatography, etc., are also reviewed.

Sampling and Analytical Method for Alpha-Dicarbonyl Flavoring Compounds via Derivatization with o-Phenylenediamine and Analysis Using GC-NPD

Directory of Open Access Journals (Sweden)

Stephanie M. Pendergrass

2016-01-01

Full Text Available A novel methodology is described for the sampling and analysis of diacetyl, 2,3-pentanedione, 2,3-hexanedione, and 2,3-heptanedione. These analytes were collected on o-phenylenediamine-treated silica gel tubes and quantitatively recovered as the corresponding quinoxaline derivatives. After derivatization, the sorbent was desorbed in 3 mL of ethanol solvent and analyzed using gas chromatography/nitrogen-phosphorous detection (GC/NPD. The limits of detection (LOD achieved for each analyte were determined to be in the range of 5–10 nanograms/sample. Evaluation of the on-tube derivatization procedure indicated that it is unaffected by humidities ranging from 20% to 80% and that the derivatization procedure was quantitative for analyte concentrations ranging from 0.1 μg to approximately 500 μg per sample. Storage stability studies indicated that the derivatives were stable for 30 days when stored at both ambient and refrigerated temperatures. Additional studies showed that the quinoxaline derivatives were quantitatively recovered when sampling up to a total volume of 72 L at a sampling rate of 50 cc/min. This method will be important to evaluate and monitor worker exposures in the food and flavoring industry. Samples can be collected over an 8-hour shift with up to 288 L total volume collected regardless of time, sampling rate, and/or the effects of humidity.

Analytical laboratory and mobile sampling platform

International Nuclear Information System (INIS)

Stetzenbach, K.; Smiecinski, A.

1996-01-01

This is the final report for the Analytical Laboratory and Mobile Sampling Platform project. This report contains only major findings and conclusions resulting from this project. Detailed reports of all activities performed for this project were provided to the Project Office every quarter since the beginning of the project. This report contains water chemistry data for samples collected in the Nevada section of Death Valley National Park (Triangle Area Springs), Nevada Test Site springs, Pahranagat Valley springs, Nevada Test Site wells, Spring Mountain springs and Crater Flat and Amargosa Valley wells

Methodological Demonstration of a Text Analytics Approach to Country Logistics System Assessments

DEFF Research Database (Denmark)

Kinra, Aseem; Mukkamala, Raghava Rao; Vatrapu, Ravi

2017-01-01

The purpose of this study is to develop and demonstrate a semi-automated text analytics approach for the identification and categorization of information that can be used for country logistics assessments. In this paper, we develop the methodology on a set of documents for 21 countries using...... and the text analyst. Implications are discussed and future work is outlined....

Quantification of analytes affected by relevant interfering signals under quality controlled conditions

International Nuclear Information System (INIS)

Bettencourt da Silva, Ricardo J.N.; Santos, Julia R.; Camoes, M. Filomena G.F.C.

2006-01-01

The analysis of organic contaminants or residues in biological samples is frequently affected by the presence of compounds producing interfering instrumental signals. This feature is responsible for the higher complexity and cost of these analyses and/or by a significant reduction of the number of studied analytes in a multi-analyte method. This work presents a methodology to estimate the impact of the interfering compounds on the quality of the analysis of complex samples, based on separative instrumental methods of analysis, aiming at supporting the inclusion of analytes affected by interfering compounds in the list of compounds analysed in the studied samples. The proposed methodology involves the study of the magnitude of the signal produced by the interfering compounds in the analysed matrix, and is applicable to analytical systems affected by interfering compounds with varying concentration in the studied matrix. The proposed methodology is based on the comparison of the signals from a representative number of examples of the studied matrix, in order to estimate the impact of the presence of such compounds on the measurement quality. The treatment of the chromatographic signals necessary to collect these data can be easily performed considering algorithms of subtraction of chromatographic signals available in most of the analytical instrumentation software. The subtraction of the interfering compounds signal from the sample signal allows the compensation of the interfering effect irrespective of the relative magnitude of the interfering and analyte signals, supporting the applicability of the same model of the method performance for a broader concentration range. The quantification of the measurement uncertainty was performed using the differential approach, which allows the estimation of the contribution of the presence of the interfering compounds to the quality of the measurement. The proposed methodology was successfully applied to the analysis of

Methodological Challenges in Examining the Impact of Healthcare Predictive Analytics on Nursing-Sensitive Patient Outcomes.

Science.gov (United States)

Jeffery, Alvin D

2015-06-01

The expansion of real-time analytic abilities within current electronic health records has led to innovations in predictive modeling and clinical decision support systems. However, the ability of these systems to influence patient outcomes is currently unknown. Even though nurses are the largest profession within the healthcare workforce, little research has been performed to explore the impact of clinical decision support on their decisions and the patient outcomes associated with them. A scoping literature review explored the impact clinical decision support systems containing healthcare predictive analytics have on four nursing-sensitive patient outcomes (pressure ulcers, failure to rescue, falls, and infections). While many articles discussed variable selection and predictive model development/validation, only four articles examined the impact on patient outcomes. The novelty of predictive analytics and the inherent methodological challenges in studying clinical decision support impact are likely responsible for this paucity of literature. Major methodological challenges include (1) multilevel nature of intervention, (2) treatment fidelity, and (3) adequacy of clinicians' subsequent behavior. There is currently insufficient evidence to demonstrate efficacy of healthcare predictive analytics-enhanced clinical decision support systems on nursing-sensitive patient outcomes. Innovative research methods and a greater emphasis on studying this phenomenon are needed.

Chapter 12. Sampling and analytical methods

International Nuclear Information System (INIS)

Busenberg, E.; Plummer, L.N.; Cook, P.G.; Solomon, D.K.; Han, L.F.; Groening, M.; Oster, H.

2006-01-01

When water samples are taken for the analysis of CFCs, regardless of the sampling method used, contamination of samples by contact with atmospheric air (with its 'high' CFC concentrations) is a major concern. This is because groundwaters usually have lower CFC concentrations than those waters which have been exposed to the modern air. Some groundwaters might not contain CFCs and, therefore, are most sensitive to trace contamination by atmospheric air. Thus, extreme precautions are needed to obtain uncontaminated samples when groundwaters, particularly those with older ages, are sampled. It is recommended at the start of any CFC investigation that samples from a CFC-free source be collected and analysed, as a check upon the sampling equipment and methodology. The CFC-free source might be a deep monitoring well or, alternatively, CFC-free water could be carefully prepared in the laboratory. It is especially important that all tubing, pumps and connection that will be used in the sampling campaign be checked in this manner

Waste minimization in analytical chemistry through innovative sample preparation techniques

International Nuclear Information System (INIS)

Smith, L. L.

1998-01-01

Because toxic solvents and other hazardous materials are commonly used in analytical methods, characterization procedures result in significant and costly amount of waste. We are developing alternative analytical methods in the radiological and organic areas to reduce the volume or form of the hazardous waste produced during sample analysis. For the radiological area, we have examined high-pressure, closed-vessel microwave digestion as a way to minimize waste from sample preparation operations. Heated solutions of strong mineral acids can be avoided for sample digestion by using the microwave approach. Because reactivity increases with pressure, we examined the use of less hazardous solvents to leach selected contaminants from soil for subsequent analysis. We demonstrated the feasibility of this approach by extracting plutonium from a NET reference material using citric and tartaric acids with microwave digestion. Analytical results were comparable to traditional digestion methods, while hazardous waste was reduced by a factor often. We also evaluated the suitability of other natural acids, determined the extraction performance on a wider variety of soil types, and examined the extraction efficiency of other contaminants. For the organic area, we examined ways to minimize the wastes associated with the determination of polychlorinated biphenyls (PCBs) in environmental samples. Conventional methods for analyzing semivolatile organic compounds are labor intensive and require copious amounts of hazardous solvents. For soil and sediment samples, we have a method to analyze PCBs that is based on microscale extraction using benign solvents (e.g., water or hexane). The extraction is performed at elevated temperatures in stainless steel cells containing the sample and solvent. Gas chromatography-mass spectrometry (GC/MS) was used to quantitate the analytes in the isolated extract. More recently, we developed a method utilizing solid-phase microextraction (SPME) for natural

Standardization of a PIGE methodology for simultaneous quantification of low Z elements in barium borosilicate glass samples

International Nuclear Information System (INIS)

Chhillar, S.; Acharya, R.; Dasari, K.B.; Pujari, P.K.; Mishra, R.K.; Kaushik, C.P.

2013-01-01

In order to standardize particle induced gamma-ray emission (PIGE) methodology for simultaneous quantification of light elements, analytical sensitivities of Li, F, B, Na, Al and Si were evaluated using 4 MeV proton beam ( ∼ 10 nA current) using 3 MV Pelletron at IOP, Bhubaneswar. The PIGE method was validated by determining all six elements in a synthetic sample in graphite matrix and applied to two barium borosilicate glass (BaBSG) samples. The prompt γ-rays emitted from inelastic scattering or nuclear reactions of corresponding isotopes were measured using a 60% HPGe coupled to MCA and the current normalized count rates were used for concentration calculation. (author)

Design of an Integrated Methodology for Analytical Design of Complex Supply Chains

Directory of Open Access Journals (Sweden)

Shahid Rashid

2012-01-01

Full Text Available A literature review and gap analysis indentifies key limitations of industry best practice when modelling of supply chains. To address these limitations the paper reports on the conception and development of an integrated modelling methodology designed to underpin the analytical design of complex supply chains. The methodology is based upon a systematic deployment of EM, CLD, and SM techniques; the integration of which is achieved via common modelling concepts and decomposition principles. Thereby the methodology facilitates: (i graphical representation and description of key “processing”, “resourcing” and “work flow” properties of supply chain configurations; (ii behavioural exploration of currently configured supply chains, to facilitate reasoning about uncertain demand impacts on supply, make, delivery, and return processes; (iii predictive quantification about relative performances of alternative complex supply chain configurations, including risk assessments. Guidelines for the application of each step of the methodology are described. Also described are recommended data collection methods and expected modelling outcomes for each step. The methodology is being extensively case tested to quantify potential benefits & costs relative to current best industry practice. The paper reflects on preliminary benefits gained during industry based case study modelling and identifies areas of potential improvement.

Analytical methodologies for broad metabolite coverage of exhaled breath condensate.

Science.gov (United States)

Aksenov, Alexander A; Zamuruyev, Konstantin O; Pasamontes, Alberto; Brown, Joshua F; Schivo, Michael; Foutouhi, Soraya; Weimer, Bart C; Kenyon, Nicholas J; Davis, Cristina E

2017-09-01

Breath analysis has been gaining popularity as a non-invasive technique that is amenable to a broad range of medical uses. One of the persistent problems hampering the wide application of the breath analysis method is measurement variability of metabolite abundances stemming from differences in both sampling and analysis methodologies used in various studies. Mass spectrometry has been a method of choice for comprehensive metabolomic analysis. For the first time in the present study, we juxtapose the most commonly employed mass spectrometry-based analysis methodologies and directly compare the resultant coverages of detected compounds in exhaled breath condensate in order to guide methodology choices for exhaled breath condensate analysis studies. Four methods were explored to broaden the range of measured compounds across both the volatile and non-volatile domain. Liquid phase sampling with polyacrylate Solid-Phase MicroExtraction fiber, liquid phase extraction with a polydimethylsiloxane patch, and headspace sampling using Carboxen/Polydimethylsiloxane Solid-Phase MicroExtraction (SPME) followed by gas chromatography mass spectrometry were tested for the analysis of volatile fraction. Hydrophilic interaction liquid chromatography and reversed-phase chromatography high performance liquid chromatography mass spectrometry were used for analysis of non-volatile fraction. We found that liquid phase breath condensate extraction was notably superior compared to headspace extraction and differences in employed sorbents manifested altered metabolite coverages. The most pronounced effect was substantially enhanced metabolite capture for larger, higher-boiling compounds using polyacrylate SPME liquid phase sampling. The analysis of the non-volatile fraction of breath condensate by hydrophilic and reverse phase high performance liquid chromatography mass spectrometry indicated orthogonal metabolite coverage by these chromatography modes. We found that the metabolite coverage

Toward decentralized analysis of mercury (II) in real samples. A critical review on nanotechnology-based methodologies

International Nuclear Information System (INIS)

Botasini, Santiago; Heijo, Gonzalo; Méndez, Eduardo

2013-01-01

Graphical abstract: -- Highlights: •Several methods based on nanotechnology achieve limit of detections in the pM and nM ranges for mercury (II) analysis. •Most of these methods are validated in filtered water samples and/or spiked samples. •Thiols in real samples constitute an actual competence for any sensor based on the binding of mercury (II) ions. •Future research should include the study of matrix interferences including thiols and dissolved organic matter. -- Abstract: In recent years, it has increased the number of works focused on the development of novel nanoparticle-based sensors for mercury detection, mainly motivated by the need of low cost portable devices capable of giving fast and reliable analytical response, thus contributing to the analytical decentralization. Methodologies employing colorimetric, fluorometric, magnetic, and electrochemical output signals allowed reaching detection limits within the pM and nM ranges. Most of these developments proved their suitability in detecting and quantifying mercury (II) ions in synthetic solutions or spiked water samples. However, the state of art in these technologies is still behind the standard methods of mercury quantification, such as cold vapor atomic absorption spectrometry and inductively coupled plasma techniques, in terms of reliability and sensitivity. This is mainly because the response of nanoparticle-based sensors is highly affected by the sample matrix. The developed analytical nanosystems may fail in real samples because of the negative incidence of the ionic strength and the presence of exchangeable ligands. The aim of this review is to critically consider the recently published innovations in this area, and highlight the needs to include more realistic assays in future research in order to make these advances suitable for on-site analysis

Comparison of soil sampling and analytical methods for asbestos at the Sumas Mountain Asbestos Site-Working towards a toolbox for better assessment.

Science.gov (United States)

Wroble, Julie; Frederick, Timothy; Frame, Alicia; Vallero, Daniel

2017-01-01

Established soil sampling methods for asbestos are inadequate to support risk assessment and risk-based decision making at Superfund sites due to difficulties in detecting asbestos at low concentrations and difficulty in extrapolating soil concentrations to air concentrations. Environmental Protection Agency (EPA)'s Office of Land and Emergency Management (OLEM) currently recommends the rigorous process of Activity Based Sampling (ABS) to characterize site exposures. The purpose of this study was to compare three soil analytical methods and two soil sampling methods to determine whether one method, or combination of methods, would yield more reliable soil asbestos data than other methods. Samples were collected using both traditional discrete ("grab") samples and incremental sampling methodology (ISM). Analyses were conducted using polarized light microscopy (PLM), transmission electron microscopy (TEM) methods or a combination of these two methods. Data show that the fluidized bed asbestos segregator (FBAS) followed by TEM analysis could detect asbestos at locations that were not detected using other analytical methods; however, this method exhibited high relative standard deviations, indicating the results may be more variable than other soil asbestos methods. The comparison of samples collected using ISM versus discrete techniques for asbestos resulted in no clear conclusions regarding preferred sampling method. However, analytical results for metals clearly showed that measured concentrations in ISM samples were less variable than discrete samples.

Analytical characterization of high-level mixed wastes using multiple sample preparation treatments

International Nuclear Information System (INIS)

King, A.G.; Baldwin, D.L.; Urie, M.W.; McKinley, S.G.

1994-01-01

The Analytical Chemistry Laboratory at the Pacific Northwest Laboratory in Richland, Washington, is actively involved in performing analytical characterization of high-level mixed waste from Hanford's single shell and double shell tank characterization programs. A full suite of analyses is typically performed on homogenized tank core samples. These analytical techniques include inductively-coupled plasma-atomic emission spectroscopy, total organic carbon methods and radiochemistry methods, as well as many others, all requiring some type of remote sample-preparation treatment to solubilize the tank sludge material for analysis. Most of these analytical methods typically use a single sample-preparation treatment, inherently providing elemental information only. To better understand and interpret tank chemistry and assist in identifying chemical compounds, selected analytical methods are performed using multiple sample-preparation treatments. The sample preparation treatments used at Pacific Northwest Laboratory for this work with high-level mixed waste include caustic fusion, acid digestion, and water leach. The type of information available by comparing results from different sample-prep treatments includes evidence for the presence of refractory compounds, acid-soluble compounds, or water-soluble compounds. Problems unique to the analysis of Hanford tank wastes are discussed. Selected results from the Hanford single shell ferrocyanide tank, 241-C-109, are presented, and the resulting conclusions are discussed

Improvements in the analytical methodology for the residue determination of the herbicide glyphosate in soils by liquid chromatography coupled to mass spectrometry.

Science.gov (United States)

Botero-Coy, A M; Ibáñez, M; Sancho, J V; Hernández, F

2013-05-31

The determination of glyphosate (GLY) in soils is of great interest due to the widespread use of this herbicide and the need of assessing its impact on the soil/water environment. However, its residue determination is very problematic especially in soils with high organic matter content, where strong interferences are normally observed, and because of the particular physico-chemical characteristics of this polar/ionic herbicide. In the present work, we have improved previous LC-MS/MS analytical methodology reported for GLY and its main metabolite AMPA in order to be applied to "difficult" soils, like those commonly found in South-America, where this herbicide is extensively used in large areas devoted to soya or maize, among other crops. The method is based on derivatization with FMOC followed by LC-MS/MS analysis, using triple quadrupole. After extraction with potassium hydroxide, a combination of extract dilution, adjustment to appropriate pH, and solid phase extraction (SPE) clean-up was applied to minimize the strong interferences observed. Despite the clean-up performed, the use of isotope labelled glyphosate as internal standard (ILIS) was necessary for the correction of matrix effects and to compensate for any error occurring during sample processing. The analytical methodology was satisfactorily validated in four soils from Colombia and Argentina fortified at 0.5 and 5mg/kg. In contrast to most LC-MS/MS methods, where the acquisition of two transitions is recommended, monitoring all available transitions was required for confirmation of positive samples, as some of them were interfered by unknown soil components. This was observed not only for GLY and AMPA but also for the ILIS. Analysis by QTOF MS was useful to confirm the presence of interferent compounds that shared the same nominal mass of analytes as well as some of their main product ions. Therefore, the selection of specific transitions was crucial to avoid interferences. The methodology developed

Identification of clinical biomarkers for pre-analytical quality control of blood samples.

Science.gov (United States)

Kang, Hyun Ju; Jeon, Soon Young; Park, Jae-Sun; Yun, Ji Young; Kil, Han Na; Hong, Won Kyung; Lee, Mee-Hee; Kim, Jun-Woo; Jeon, Jae-Pil; Han, Bok Ghee

2013-04-01

Pre-analytical conditions are key factors in maintaining the high quality of biospecimens. They are necessary for accurate reproducibility of experiments in the field of biomarker discovery as well as achieving optimal specificity of laboratory tests for clinical diagnosis. In research at the National Biobank of Korea, we evaluated the impact of pre-analytical conditions on the stability of biobanked blood samples by measuring biochemical analytes commonly used in clinical laboratory tests. We measured 10 routine laboratory analytes in serum and plasma samples from healthy donors (n = 50) with a chemistry autoanalyzer (Hitachi 7600-110). The analyte measurements were made at different time courses based on delay of blood fractionation, freezing delay of fractionated serum and plasma samples, and at different cycles (0, 1, 3, 6, 9) of freeze-thawing. Statistically significant changes from the reference sample mean were determined using the repeated-measures ANOVA and the significant change limit (SCL). The serum levels of GGT and LDH were changed significantly depending on both the time interval between blood collection and fractionation and the time interval between fractionation and freezing of serum and plasma samples. The glucose level was most sensitive only to the elapsed time between blood collection and centrifugation for blood fractionation. Based on these findings, a simple formula (glucose decrease by 1.387 mg/dL per hour) was derived to estimate the length of time delay after blood collection. In addition, AST, BUN, GGT, and LDH showed sensitive responses to repeated freeze-thaw cycles of serum and plasma samples. These results suggest that GGT and LDH measurements can be used as quality control markers for certain pre-analytical conditions (eg, delayed processing or repeated freeze-thawing) of blood samples which are either directly used in the laboratory tests or stored for future research in the biobank.

Evidential analytic hierarchy process dependence assessment methodology in human reliability analysis

International Nuclear Information System (INIS)

Chen, Lu Yuan; Zhou, Xinyi; Xiao, Fuyuan; Deng, Yong; Mahadevan, Sankaran

2017-01-01

In human reliability analysis, dependence assessment is an important issue in risky large complex systems, such as operation of a nuclear power plant. Many existing methods depend on an expert's judgment, which contributes to the subjectivity and restrictions of results. Recently, a computational method, based on the Dempster-Shafer evidence theory and analytic hierarchy process, has been proposed to handle the dependence in human reliability analysis. The model can deal with uncertainty in an analyst's judgment and reduce the subjectivity in the evaluation process. However, the computation is heavy and complicated to some degree. The most important issue is that the existing method is in a positive aspect, which may cause an underestimation of the risk. In this study, a new evidential analytic hierarchy process dependence assessment methodology, based on the improvement of existing methods, has been proposed, which is expected to be easier and more effective

Evidential Analytic Hierarchy Process Dependence Assessment Methodology in Human Reliability Analysis

Directory of Open Access Journals (Sweden)

Luyuan Chen

2017-02-01

Full Text Available In human reliability analysis, dependence assessment is an important issue in risky large complex systems, such as operation of a nuclear power plant. Many existing methods depend on an expert's judgment, which contributes to the subjectivity and restrictions of results. Recently, a computational method, based on the Dempster–Shafer evidence theory and analytic hierarchy process, has been proposed to handle the dependence in human reliability analysis. The model can deal with uncertainty in an analyst's judgment and reduce the subjectivity in the evaluation process. However, the computation is heavy and complicated to some degree. The most important issue is that the existing method is in a positive aspect, which may cause an underestimation of the risk. In this study, a new evidential analytic hierarchy process dependence assessment methodology, based on the improvement of existing methods, has been proposed, which is expected to be easier and more effective.

Evidential analytic hierarchy process dependence assessment methodology in human reliability analysis

Energy Technology Data Exchange (ETDEWEB)

Chen, Lu Yuan; Zhou, Xinyi; Xiao, Fuyuan; Deng, Yong [School of Computer and Information Science, Southwest University, Chongqing (China); Mahadevan, Sankaran [School of Engineering, Vanderbilt University, Nashville (United States)

2017-02-15

In human reliability analysis, dependence assessment is an important issue in risky large complex systems, such as operation of a nuclear power plant. Many existing methods depend on an expert's judgment, which contributes to the subjectivity and restrictions of results. Recently, a computational method, based on the Dempster-Shafer evidence theory and analytic hierarchy process, has been proposed to handle the dependence in human reliability analysis. The model can deal with uncertainty in an analyst's judgment and reduce the subjectivity in the evaluation process. However, the computation is heavy and complicated to some degree. The most important issue is that the existing method is in a positive aspect, which may cause an underestimation of the risk. In this study, a new evidential analytic hierarchy process dependence assessment methodology, based on the improvement of existing methods, has been proposed, which is expected to be easier and more effective.

Preparation of standard hair material and development of analytical methodology

International Nuclear Information System (INIS)

Gangadharan, S.; Ganapathi Iyer, S.; Ali, M.M.; Thantry, S.S.; Verma, R.; Arunachalam, J.; Walvekar, A.P.

1992-01-01

In 1976 Indian Researchers suggested the possible use of hair as an indicator of environmental exposure and established through a study of country wide student population and general population of the metropolitan city of Bombay that human scalp hair could indeed be an effective first level monitor in a scheme of multilevel monitoring of environmental exposure to inorganic pollutants. It was in this context and in view of the ready availability of large quantities of scalp hair subjected to minimum treatment by chemicals that they proposed to participate in the preparation of a standard material of hair. It was also recognized that measurements of trace element concentrations at very low levels require cross-validation by different analytical techniques, even within the same laboratory. The programme of work that has been carried out since the first meeting of the CRP had been aimed at these two objectives. These objectives include the preparation of standard material of hair and the development of analytical methodologies for determination of elements and species of interest. 1 refs., 3 tabs

Protocols for the analytical characterization of therapeutic monoclonal antibodies. II - Enzymatic and chemical sample preparation.

Science.gov (United States)

Bobaly, Balazs; D'Atri, Valentina; Goyon, Alexandre; Colas, Olivier; Beck, Alain; Fekete, Szabolcs; Guillarme, Davy

2017-08-15

The analytical characterization of therapeutic monoclonal antibodies and related proteins usually incorporates various sample preparation methodologies. Indeed, quantitative and qualitative information can be enhanced by simplifying the sample, thanks to the removal of sources of heterogeneity (e.g. N-glycans) and/or by decreasing the molecular size of the tested protein by enzymatic or chemical fragmentation. These approaches make the sample more suitable for chromatographic and mass spectrometric analysis. Structural elucidation and quality control (QC) analysis of biopharmaceutics are usually performed at intact, subunit and peptide levels. In this paper, general sample preparation approaches used to attain peptide, subunit and glycan level analysis are overviewed. Protocols are described to perform tryptic proteolysis, IdeS and papain digestion, reduction as well as deglycosylation by PNGase F and EndoS2 enzymes. Both historical and modern sample preparation methods were compared and evaluated using rituximab and trastuzumab, two reference therapeutic mAb products approved by Food and Drug Administration (FDA) and European Medicines Agency (EMA). The described protocols may help analysts to develop sample preparation methods in the field of therapeutic protein analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

Analytical methodologies for the determination of nutraceuticals in foods

International Nuclear Information System (INIS)

Rosanna, Gatti; Domenica Masci

2015-01-01

The term nutraceutical was coined almost thirty years ago (Stephen De Felice, 1989) by the union of the two terms nutrition and pharmaceutical. According to the definition, for 'Nutraceutical' refers to 'any substance that can be considered a food (or part of a food), and which provides medical or health benefits, including the prevention and / or the treatment of a disease'. At the Casaccia Research Centre ENEA, are developed and validated methodologies analytics for detection and quantification of nutraceutical substances. This is to highlight some cultivars in relation to genotype, geographical area production, cultural practices, or for the purpose to assess the content relative to conservation techniques or transport of raw materials and processed products. [it

Sampling and analyte enrichment strategies for ambient mass spectrometry.

Science.gov (United States)

Li, Xianjiang; Ma, Wen; Li, Hongmei; Ai, Wanpeng; Bai, Yu; Liu, Huwei

2018-01-01

Ambient mass spectrometry provides great convenience for fast screening, and has showed promising potential in analytical chemistry. However, its relatively low sensitivity seriously restricts its practical utility in trace compound analysis. In this review, we summarize the sampling and analyte enrichment strategies coupled with nine modes of representative ambient mass spectrometry (desorption electrospray ionization, paper vhspray ionization, wooden-tip spray ionization, probe electrospray ionization, coated blade spray ionization, direct analysis in real time, desorption corona beam ionization, dielectric barrier discharge ionization, and atmospheric-pressure solids analysis probe) that have dramatically increased the detection sensitivity. We believe that these advances will promote routine use of ambient mass spectrometry. Graphical abstract Scheme of sampling stretagies for ambient mass spectrometry.

Novel methodology to isolate microplastics from vegetal-rich samples.

Science.gov (United States)

Herrera, Alicia; Garrido-Amador, Paloma; Martínez, Ico; Samper, María Dolores; López-Martínez, Juan; Gómez, May; Packard, Theodore T

2018-04-01

Microplastics are small plastic particles, globally distributed throughout the oceans. To properly study them, all the methodologies for their sampling, extraction, and measurement should be standardized. For heterogeneous samples containing sediments, animal tissues and zooplankton, several procedures have been described. However, definitive methodologies for samples, rich in algae and plant material, have not yet been developed. The aim of this study was to find the best extraction protocol for vegetal-rich samples by comparing the efficacies of five previously described digestion methods, and a novel density separation method. A protocol using 96% ethanol for density separation was better than the five digestion methods tested, even better than using H 2 O 2 digestion. As it was the most efficient, simple, safe and inexpensive method for isolating microplastics from vegetal rich samples, we recommend it as a standard separation method. Copyright © 2018 Elsevier Ltd. All rights reserved.

Analytical Methodologies for the Stereoselective Determination of Sibutramine: An Overview

Directory of Open Access Journals (Sweden)

Vlad Alexandru Robert

2017-06-01

Full Text Available Sibutramine is a chiral anti-obesity drug which decreases food intake and increases energy expenditure. In therapy it is used as a racemic mixture; however both pharmacokinetic and pharmacodynamic data have revealed enantioselective behavior of sibutramine and its major active metabolites. Several chromatographic and electrophoretic analytical methods have been published so far for the chiral determination of sibutramine from pharmaceutical preparations and biological samples. The current paper aims to provide a systematic review of the stereochemical aspects and analytical methods used for the enantiodetermination of sibutramine and its active enantiomers covering the last 15 years.

Green sample preparation for liquid chromatography and capillary electrophoresis of anionic and cationic analytes.

Science.gov (United States)

Wuethrich, Alain; Haddad, Paul R; Quirino, Joselito P

2015-04-21

A sample preparation device for the simultaneous enrichment and separation of cationic and anionic analytes was designed and implemented in an eight-channel configuration. The device is based on the use of an electric field to transfer the analytes from a large volume of sample into small volumes of electrolyte that was suspended into two glass micropipettes using a conductive hydrogel. This simple, economical, fast, and green (no organic solvent required) sample preparation scheme was evaluated using cationic and anionic herbicides as test analytes in water. The analytical figures of merit and ecological aspects were evaluated against the state-of-the-art sample preparation, solid-phase extraction. A drastic reduction in both sample preparation time (94% faster) and resources (99% less consumables used) was observed. Finally, the technique in combination with high-performance liquid chromatography and capillary electrophoresis was applied to analysis of quaternary ammonium and phenoxypropionic acid herbicides in fortified river water as well as drinking water (at levels relevant to Australian guidelines). The presented sustainable sample preparation approach could easily be applied to other charged analytes or adopted by other laboratories.

A sample preparation method for recovering suppressed analyte ions in MALDI TOF MS

NARCIS (Netherlands)

Lou, X.; Waal, de B.F.M.; Milroy, L.G.; Dongen, van J.L.J.

2015-01-01

In matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI TOF MS), analyte signals can be substantially suppressed by other compounds in the sample. In this technical note, we describe a modified thin-layer sample preparation method that significantly reduces the analyte

OPTIMAL METHOD FOR PREPARATION OF SILICATE ROCK SAMPLES FOR ANALYTICAL PURPOSES

Directory of Open Access Journals (Sweden)

Maja Vrkljan

2004-12-01

Full Text Available The purpose of this study was to determine an optimal dissolution method for silicate rock samples for further analytical purposes. Analytical FAAS method of determining cobalt, chromium, copper, nickel, lead and zinc content in gabbro sample and geochemical standard AGV-1 has been applied for verification. Dissolution in mixtures of various inorganic acids has been tested, as well as Na2CO3 fusion technique. The results obtained by different methods have been compared and dissolution in the mixture of HNO3 + HF has been recommended as optimal.

Green approaches in sample preparation of bioanalytical samples prior to chromatographic analysis.

Science.gov (United States)

Filippou, Olga; Bitas, Dimitrios; Samanidou, Victoria

2017-02-01

Sample preparation is considered to be the most challenging step of the analytical procedure, since it has an effect on the whole analytical methodology, therefore it contributes significantly to the greenness or lack of it of the entire process. The elimination of the sample treatment steps, pursuing at the same time the reduction of the amount of the sample, strong reductions in consumption of hazardous reagents and energy also maximizing safety for operators and environment, the avoidance of the use of big amount of organic solvents, form the basis for greening sample preparation and analytical methods. In the last decade, the development and utilization of greener and sustainable microextraction techniques is an alternative to classical sample preparation procedures. In this review, the main green microextraction techniques (solid phase microextraction, stir bar sorptive extraction, hollow-fiber liquid phase microextraction, dispersive liquid - liquid microextraction, etc.) will be presented, with special attention to bioanalytical applications of these environment-friendly sample preparation techniques which comply with the green analytical chemistry principles. Copyright © 2016 Elsevier B.V. All rights reserved.

Recent developments and future trends in solid phase microextraction techniques towards green analytical chemistry.

Science.gov (United States)

Spietelun, Agata; Marcinkowski, Łukasz; de la Guardia, Miguel; Namieśnik, Jacek

2013-12-20

Solid phase microextraction find increasing applications in the sample preparation step before chromatographic determination of analytes in samples with a complex composition. These techniques allow for integrating several operations, such as sample collection, extraction, analyte enrichment above the detection limit of a given measuring instrument and the isolation of analytes from sample matrix. In this work the information about novel methodological and instrumental solutions in relation to different variants of solid phase extraction techniques, solid-phase microextraction (SPME), stir bar sorptive extraction (SBSE) and magnetic solid phase extraction (MSPE) is presented, including practical applications of these techniques and a critical discussion about their advantages and disadvantages. The proposed solutions fulfill the requirements resulting from the concept of sustainable development, and specifically from the implementation of green chemistry principles in analytical laboratories. Therefore, particular attention was paid to the description of possible uses of novel, selective stationary phases in extraction techniques, inter alia, polymeric ionic liquids, carbon nanotubes, and silica- and carbon-based sorbents. The methodological solutions, together with properly matched sampling devices for collecting analytes from samples with varying matrix composition, enable us to reduce the number of errors during the sample preparation prior to chromatographic analysis as well as to limit the negative impact of this analytical step on the natural environment and the health of laboratory employees. Copyright © 2013 Elsevier B.V. All rights reserved.

Large sample NAA facility and methodology development

International Nuclear Information System (INIS)

Roth, C.; Gugiu, D.; Barbos, D.; Datcu, A.; Aioanei, L.; Dobrea, D.; Taroiu, I. E.; Bucsa, A.; Ghinescu, A.

2013-01-01

A Large Sample Neutron Activation Analysis (LSNAA) facility has been developed at the TRIGA- Annular Core Pulsed Reactor (ACPR) operated by the Institute for Nuclear Research in Pitesti, Romania. The central irradiation cavity of the ACPR core can accommodate a large irradiation device. The ACPR neutron flux characteristics are well known and spectrum adjustment techniques have been successfully applied to enhance the thermal component of the neutron flux in the central irradiation cavity. An analysis methodology was developed by using the MCNP code in order to estimate counting efficiency and correction factors for the major perturbing phenomena. Test experiments, comparison with classical instrumental neutron activation analysis (INAA) methods and international inter-comparison exercise have been performed to validate the new methodology. (authors)

Analytical study on the determination of boron in environmental water samples

International Nuclear Information System (INIS)

Lopez, F.J.; Gimenez, E.; Hernandez, F.

1993-01-01

An analytical study on the determination of boron in environmental water samples was carried out. The curcumin and carmine standard methods were compared with the most recent Azomethine-H method in order to evaluate their analytical characteristics and feasibility for the analysis of boron in water samples. Analyses of synthetic water, ground water, sea water and waste water samples were carried out and a statistical evaluation of the results was made. The Azomethine-H method was found to be the most sensitive (detection limit 0.02 mg l -1 ) and selective (no interference of commonly occurring ions in water was observed), showing also the best precision (relative standard deviation lower than 4%). Moreover, it gave good results for all types of samples analyzed. The accuracy of this method was tested by the addition of known amounts of standard solutions to different types of water samples. The slopes of standard additions and direct calibration graphs were similar and recoveries of added boron ranged from 99 to 107%. (orig.)

Temperature-controlled micro-TLC: a versatile green chemistry and fast analytical tool for separation and preliminary screening of steroids fraction from biological and environmental samples.

Science.gov (United States)

Zarzycki, Paweł K; Slączka, Magdalena M; Zarzycka, Magdalena B; Bartoszuk, Małgorzata A; Włodarczyk, Elżbieta; Baran, Michał J

2011-11-01

This paper is a continuation of our previous research focusing on development of micro-TLC methodology under temperature-controlled conditions. The main goal of present paper is to demonstrate separation and detection capability of micro-TLC technique involving simple analytical protocols without multi-steps sample pre-purification. One of the advantages of planar chromatography over its column counterpart is that each TLC run can be performed using non-previously used stationary phase. Therefore, it is possible to fractionate or separate complex samples characterized by heavy biological matrix loading. In present studies components of interest, mainly steroids, were isolated from biological samples like fish bile using single pre-treatment steps involving direct organic liquid extraction and/or deproteinization by freeze-drying method. Low-molecular mass compounds with polarity ranging from estetrol to progesterone derived from the environmental samples (lake water, untreated and treated sewage waters) were concentrated using optimized solid-phase extraction (SPE). Specific bands patterns for samples derived from surface water of the Middle Pomerania in northern part of Poland can be easily observed on obtained micro-TLC chromatograms. This approach can be useful as simple and non-expensive complementary method for fast control and screening of treated sewage water discharged by the municipal wastewater treatment plants. Moreover, our experimental results show the potential of micro-TLC as an efficient tool for retention measurements of a wide range of steroids under reversed-phase (RP) chromatographic conditions. These data can be used for further optimalization of SPE or HPLC systems working under RP conditions. Furthermore, we also demonstrated that micro-TLC based analytical approach can be applied as an effective method for the internal standard (IS) substance search. Generally, described methodology can be applied for fast fractionation or screening of the

Metal-organic frameworks for analytical chemistry: from sample collection to chromatographic separation.

Science.gov (United States)

Gu, Zhi-Yuan; Yang, Cheng-Xiong; Chang, Na; Yan, Xiu-Ping

2012-05-15

In modern analytical chemistry researchers pursue novel materials to meet analytical challenges such as improvements in sensitivity, selectivity, and detection limit. Metal-organic frameworks (MOFs) are an emerging class of microporous materials, and their unusual properties such as high surface area, good thermal stability, uniform structured nanoscale cavities, and the availability of in-pore functionality and outer-surface modification are attractive for diverse analytical applications. This Account summarizes our research on the analytical applications of MOFs ranging from sampling to chromatographic separation. MOFs have been either directly used or engineered to meet the demands of various analytical applications. Bulk MOFs with microsized crystals are convenient sorbents for direct application to in-field sampling and solid-phase extraction. Quartz tubes packed with MOF-5 have shown excellent stability, adsorption efficiency, and reproducibility for in-field sampling and trapping of atmospheric formaldehyde. The 2D copper(II) isonicotinate packed microcolumn has demonstrated large enhancement factors and good shape- and size-selectivity when applied to on-line solid-phase extraction of polycyclic aromatic hydrocarbons in water samples. We have explored the molecular sieving effect of MOFs for the efficient enrichment of peptides with simultaneous exclusion of proteins from biological fluids. These results show promise for the future of MOFs in peptidomics research. Moreover, nanosized MOFs and engineered thin films of MOFs are promising materials as novel coatings for solid-phase microextraction. We have developed an in situ hydrothermal growth approach to fabricate thin films of MOF-199 on etched stainless steel wire for solid-phase microextraction of volatile benzene homologues with large enhancement factors and wide linearity. Their high thermal stability and easy-to-engineer nanocrystals make MOFs attractive as new stationary phases to fabricate MOF

105-N Basin sediment disposition phase-one sampling and analysis plan

International Nuclear Information System (INIS)

1997-01-01

The sampling and analysis plan (SAP) for Phase 1 of the 105-N Basin sediment disposition project defines the sampling and analytical activities that will be performed for the engineering assessment phase (phase 1) of the project. A separate SAP defines the sampling and analytical activities that will be performed for the characterization phase (Phase 2) of the 105-N sediment disposition project. The Phase-1 SAP is presented in the introduction (Section 1.0), in the field sampling plan (FSP) (Section 2.0), and in the quality assurance project plan (QAPjP) (Section 3.0). The FSP defines the sampling and analytical methodologies to be performed. The QAPjP provides information on the quality assurance/quality control (QA/QC) parameters related to the sampling and analytical methodologies. This SAP defines the strategy and the methods that will be used to sample and analyze the sediment on the floor of the 105-N Basin. The resulting data will be used to develop and evaluate engineering designs for collecting and removing sediment from the basin

FIGURED WORLDS AS AN ANALYTIC AND METHODOLOGICAL TOOL IN PROFESSIONAL TEACHER DEVELOPMENT

DEFF Research Database (Denmark)

Møller, Hanne; Brok, Lene Storgaard

. Hasse (2015) and Holland (1998) have inspired our study; i.e., learning is conceptualized as a social phenomenon, implying that contexts of learning are decisive for learner identity. The concept of Figured Worlds is used to understand the development and the social constitution of emergent interactions......,“(Holland et al., 1998, p. 52) and gives a framework for understanding meaning-making in particular pedagogical settings. We exemplify our use of the term Figured Worlds, both as an analytic and methodological tool for empirical studies in kindergarten and school. Based on data sources, such as field notes...

Methodological procedures and analytical instruments to evaluate an indicators integrated archive for urban management

International Nuclear Information System (INIS)

Del Ciello, R.; Napoleoni, S.

1998-01-01

This guide provides the results of a research developed at ENEA (National Agency for new Technology, Energy and the Environment) Casaccia center (Rome, Italy) aimed to define methodological procedures and analytical instruments needed to carry out an indicators integrated archive for urban management. The guide also defines the scheme of a negotiation process aimed to reach and exchange data and information among governmental and local administrations, non-governmental organizations and scientific bodies [it

Analytical methodology for optimization of waste management scenarios in nuclear installation decommissioning process - 16148

International Nuclear Information System (INIS)

Zachar, Matej; Necas, Vladimir; Daniska, Vladimir; Rehak, Ivan; Vasko, Marek

2009-01-01

The nuclear installation decommissioning process is characterized by production of large amount of various radioactive and non-radioactive waste that has to be managed, taking into account its physical, chemical, toxic and radiological properties. Waste management is considered to be one of the key issues within the frame of the decommissioning process. During the decommissioning planning period, the scenarios covering possible routes of materials release into the environment and radioactive waste disposal, should be discussed and evaluated. Unconditional and conditional release to the environment, long-term storage at the nuclear site, near surface or deep geological disposal and relevant material management techniques for achieving the final status should be taken into account in the analysed scenarios. At the level of the final decommissioning plan, it is desirable to have the waste management scenario optimized for local specific facility conditions taking into account a national decommissioning background. The analytical methodology for the evaluation of decommissioning waste management scenarios, presented in the paper, is based on the materials and radioactivity flow modelling, which starts from waste generation activities like pre-dismantling decontamination, selected methods of dismantling, waste treatment and conditioning, up to materials release or conditioned radioactive waste disposal. The necessary input data for scenarios, e.g. nuclear installation inventory database (physical and radiological data), waste processing technologies parameters or material release and waste disposal limits, have to be considered. The analytical methodology principles are implemented into the standardised decommissioning parameters calculation code OMEGA, developed in the DECOM company. In the paper the examples of the methodology implementation for the scenarios optimization are presented and discussed. (authors)

Multi-model approach to petroleum resource appraisal using analytic methodologies for probabilistic systems

Science.gov (United States)

Crovelli, R.A.

1988-01-01

The geologic appraisal model that is selected for a petroleum resource assessment depends upon purpose of the assessment, basic geologic assumptions of the area, type of available data, time available before deadlines, available human and financial resources, available computer facilities, and, most importantly, the available quantitative methodology with corresponding computer software and any new quantitative methodology that would have to be developed. Therefore, different resource assessment projects usually require different geologic models. Also, more than one geologic model might be needed in a single project for assessing different regions of the study or for cross-checking resource estimates of the area. Some geologic analyses used in the past for petroleum resource appraisal involved play analysis. The corresponding quantitative methodologies of these analyses usually consisted of Monte Carlo simulation techniques. A probabilistic system of petroleum resource appraisal for play analysis has been designed to meet the following requirements: (1) includes a variety of geologic models, (2) uses an analytic methodology instead of Monte Carlo simulation, (3) possesses the capacity to aggregate estimates from many areas that have been assessed by different geologic models, and (4) runs quickly on a microcomputer. Geologic models consist of four basic types: reservoir engineering, volumetric yield, field size, and direct assessment. Several case histories and present studies by the U.S. Geological Survey are discussed. ?? 1988 International Association for Mathematical Geology.

Detection, characterization and quantification of inorganic engineered nanomaterials: A review of techniques and methodological approaches for the analysis of complex samples

Energy Technology Data Exchange (ETDEWEB)

Laborda, Francisco, E-mail: flaborda@unizar.es; Bolea, Eduardo; Cepriá, Gemma; Gómez, María T.; Jiménez, María S.; Pérez-Arantegui, Josefina; Castillo, Juan R.

2016-01-21

The increasing demand of analytical information related to inorganic engineered nanomaterials requires the adaptation of existing techniques and methods, or the development of new ones. The challenge for the analytical sciences has been to consider the nanoparticles as a new sort of analytes, involving both chemical (composition, mass and number concentration) and physical information (e.g. size, shape, aggregation). Moreover, information about the species derived from the nanoparticles themselves and their transformations must also be supplied. Whereas techniques commonly used for nanoparticle characterization, such as light scattering techniques, show serious limitations when applied to complex samples, other well-established techniques, like electron microscopy and atomic spectrometry, can provide useful information in most cases. Furthermore, separation techniques, including flow field flow fractionation, capillary electrophoresis and hydrodynamic chromatography, are moving to the nano domain, mostly hyphenated to inductively coupled plasma mass spectrometry as element specific detector. Emerging techniques based on the detection of single nanoparticles by using ICP-MS, but also coulometry, are in their way to gain a position. Chemical sensors selective to nanoparticles are in their early stages, but they are very promising considering their portability and simplicity. Although the field is in continuous evolution, at this moment it is moving from proofs-of-concept in simple matrices to methods dealing with matrices of higher complexity and relevant analyte concentrations. To achieve this goal, sample preparation methods are essential to manage such complex situations. Apart from size fractionation methods, matrix digestion, extraction and concentration methods capable of preserving the nature of the nanoparticles are being developed. This review presents and discusses the state-of-the-art analytical techniques and sample preparation methods suitable for

Detection, characterization and quantification of inorganic engineered nanomaterials: A review of techniques and methodological approaches for the analysis of complex samples

International Nuclear Information System (INIS)

Laborda, Francisco; Bolea, Eduardo; Cepriá, Gemma; Gómez, María T.; Jiménez, María S.; Pérez-Arantegui, Josefina; Castillo, Juan R.

2016-01-01

The increasing demand of analytical information related to inorganic engineered nanomaterials requires the adaptation of existing techniques and methods, or the development of new ones. The challenge for the analytical sciences has been to consider the nanoparticles as a new sort of analytes, involving both chemical (composition, mass and number concentration) and physical information (e.g. size, shape, aggregation). Moreover, information about the species derived from the nanoparticles themselves and their transformations must also be supplied. Whereas techniques commonly used for nanoparticle characterization, such as light scattering techniques, show serious limitations when applied to complex samples, other well-established techniques, like electron microscopy and atomic spectrometry, can provide useful information in most cases. Furthermore, separation techniques, including flow field flow fractionation, capillary electrophoresis and hydrodynamic chromatography, are moving to the nano domain, mostly hyphenated to inductively coupled plasma mass spectrometry as element specific detector. Emerging techniques based on the detection of single nanoparticles by using ICP-MS, but also coulometry, are in their way to gain a position. Chemical sensors selective to nanoparticles are in their early stages, but they are very promising considering their portability and simplicity. Although the field is in continuous evolution, at this moment it is moving from proofs-of-concept in simple matrices to methods dealing with matrices of higher complexity and relevant analyte concentrations. To achieve this goal, sample preparation methods are essential to manage such complex situations. Apart from size fractionation methods, matrix digestion, extraction and concentration methods capable of preserving the nature of the nanoparticles are being developed. This review presents and discusses the state-of-the-art analytical techniques and sample preparation methods suitable for

Determination of 237Np in environmental and nuclear samples: A review of the analytical method

International Nuclear Information System (INIS)

Thakur, P.; Mulholland, G.P.

2012-01-01

A number of analytical methods has been developed and used for the determination of neptunium in environmental and nuclear fuel samples using alpha, ICP–MS spectrometry, and other analytical techniques. This review summarizes and discusses development of the radiochemical procedures for separation of neptunium (Np), since the beginning of the nuclear industry, followed by a more detailed discussion on recent trends in the separation of neptunium. This article also highlights the progress in analytical methods and issues associated with the determination of neptunium in environmental samples. - Highlights: ► Determination of Np in environmental and nuclear samples is reviewed. ► Various analytical methods used for the determination of Np are listed. ► Progress and issues associated with the determination of Np are discussed.

Pre-analytical sample quality: metabolite ratios as an intrinsic marker for prolonged room temperature exposure of serum samples.

Directory of Open Access Journals (Sweden)

Gabriele Anton

Full Text Available Advances in the "omics" field bring about the need for a high number of good quality samples. Many omics studies take advantage of biobanked samples to meet this need. Most of the laboratory errors occur in the pre-analytical phase. Therefore evidence-based standard operating procedures for the pre-analytical phase as well as markers to distinguish between 'good' and 'bad' quality samples taking into account the desired downstream analysis are urgently needed. We studied concentration changes of metabolites in serum samples due to pre-storage handling conditions as well as due to repeated freeze-thaw cycles. We collected fasting serum samples and subjected aliquots to up to four freeze-thaw cycles and to pre-storage handling delays of 12, 24 and 36 hours at room temperature (RT and on wet and dry ice. For each treated aliquot, we quantified 127 metabolites through a targeted metabolomics approach. We found a clear signature of degradation in samples kept at RT. Storage on wet ice led to less pronounced concentration changes. 24 metabolites showed significant concentration changes at RT. In 22 of these, changes were already visible after only 12 hours of storage delay. Especially pronounced were increases in lysophosphatidylcholines and decreases in phosphatidylcholines. We showed that the ratio between the concentrations of these molecule classes could serve as a measure to distinguish between 'good' and 'bad' quality samples in our study. In contrast, we found quite stable metabolite concentrations during up to four freeze-thaw cycles. We concluded that pre-analytical RT handling of serum samples should be strictly avoided and serum samples should always be handled on wet ice or in cooling devices after centrifugation. Moreover, serum samples should be frozen at or below -80°C as soon as possible after centrifugation.

Determination of trace impurities in uranium-transition metal alloy fuels by ICP-MS using extended common analyte internal standardization (ECAIS) technique

International Nuclear Information System (INIS)

Saha, Abhijit; Deb, S.B.; Nagar, B.K.; Saxena, M.K.

2015-01-01

An analytical methodology was developed for the determination of eight trace impurities viz, Al, B, Cd, Co, Cu, Mg, Mn and Ni in three different uranium-transition metal alloy fuels (U-Me; Me = Ti, Zr and Mo) employing inductively coupled plasma mass spectrometry (ICP-MS). The well known common analyte internal standardization (CAIS) chemometric technique was modified and then employed to minimize and account for the matrix effect on analyte intensity. Standard addition of analytes to the pure synthetic U-Me sample solutions and subsequently their ≥ 94% recovery by the ICP-MS measurement validates the proposed methodology. One real sample of each of these alloys was analyzed by the developed analytical methodology and the %RSD observed was in the range of 5-8%. The method detection limits were found to be within 4-10 μg L -1 . (author)

Analytical characterization using surface-enhanced Raman scattering (SERS) and microfluidic sampling

International Nuclear Information System (INIS)

Wang, Chao; Yu, Chenxu

2015-01-01

With the rapid development of analytical techniques, it has become much easier to detect chemical and biological analytes, even at very low detection limits. In recent years, techniques based on vibrational spectroscopy, such as surface enhanced Raman spectroscopy (SERS), have been developed for non-destructive detection of pathogenic microorganisms. SERS is a highly sensitive analytical tool that can be used to characterize chemical and biological analytes interacting with SERS-active substrates. However, it has always been a challenge to obtain consistent and reproducible SERS spectroscopic results at complicated experimental conditions. Microfluidics, a tool for highly precise manipulation of small volume liquid samples, can be used to overcome the major drawbacks of SERS-based techniques. High reproducibility of SERS measurement could be obtained in continuous flow generated inside microfluidic devices. This article provides a thorough review of the principles, concepts and methods of SERS-microfluidic platforms, and the applications of such platforms in trace analysis of chemical and biological analytes. (topical review)

Analytical simulation of RBS spectra of nanowire samples

Energy Technology Data Exchange (ETDEWEB)

Barradas, Nuno P., E-mail: nunoni@ctn.ist.utl.pt [Centro de Ciências e Tecnologias Nucleares, Instituto Superior Técnico, Universidade de Lisboa, E.N. 10 ao km 139,7, 2695-066 Bobadela LRS (Portugal); García Núñez, C. [Laboratorio de Electrónica y Semiconductores, Departamento de Física Aplicada, Universidad Autónoma de Madrid, 28049 Madrid (Spain); Redondo-Cubero, A. [Laboratorio de Electrónica y Semiconductores, Departamento de Física Aplicada, Universidad Autónoma de Madrid, 28049 Madrid (Spain); Centro de Micro-Análisis de Materiales, Universidad Autónoma de Madrid, 28049 Madrid (Spain); Shen, G.; Kung, P. [Department of Electrical and Computer Engineering, The University of Alabama, AL 35487 (United States); Pau, J.L. [Laboratorio de Electrónica y Semiconductores, Departamento de Física Aplicada, Universidad Autónoma de Madrid, 28049 Madrid (Spain)

2016-03-15

Almost all, if not all, general purpose codes for analysis of Ion Beam Analysis data have been originally developed to handle laterally homogeneous samples only. This is the case of RUMP, NDF, SIMNRA, and even of the Monte Carlo code Corteo. General-purpose codes usually include only limited support for lateral inhomogeneity. In this work, we show analytical simulations of samples that consist of a layer of parallel oriented nanowires on a substrate, using a model implemented in NDF. We apply the code to real samples, made of vertical ZnO nanowires on a sapphire substrate. Two configurations of the nanowires were studied: 40 nm diameter, 4.1 μm height, 3.5% surface coverage; and 55 nm diameter, 1.1 μm height, 42% surface coverage. We discuss the accuracy and limits of applicability of the analysis.

Radiochemical methodologies applied to analytical characterization of low and intermediate level wastes from nuclear power plants

International Nuclear Information System (INIS)

Monteiro, Roberto Pellacani G.; Júnior, Aluísio Souza R.; Kastner, Geraldo F.; Temba, Eliane S.C.; Oliveira, Thiago C. de; Amaral, Ângela M.; Franco, Milton B.

2017-01-01

The aim of this work is to present radiochemical methodologies developed at CDTN/CNEN in order to answer a program for isotopic inventory of radioactive wastes from Brazilian Nuclear Power Plants. In this program some radionuclides, 3 H, 14 C, 55 Fe, 59 Ni, 63 Ni, 90 Sr, 93 Zr, 94 Nb, 99 Tc, 129 I, 235 U, 238 U, 238 Pu, 239 + 240 Pu, 241 Pu, 242 Pu, 241 Am, 242 Cm e 243 + 244 Cm, were determined in Low Level Wastes (LLW) and Intermediate Level Wastes (ILW) and a protocol of analytical methodologies based on radiochemical separation steps and spectrometric and nuclear techniques was established. (author)

Tank 214-AW-105, grab samples, analytical results for the final report

International Nuclear Information System (INIS)

Esch, R.A.

1997-01-01

This document is the final report for tank 241-AW-105 grab samples. Twenty grabs samples were collected from risers 10A and 15A on August 20 and 21, 1996, of which eight were designated for the K Basin sludge compatibility and mixing studies. This document presents the analytical results for the remaining twelve samples. Analyses were performed in accordance with the Compatibility Grab Sampling and Analysis Plan (TSAP) and the Data Quality Objectives for Tank Farms Waste Compatibility Program (DO). The results for the previous sampling of this tank were reported in WHC-SD-WM-DP-149, Rev. 0, 60-Day Waste Compatibility Safety Issue and Final Results for Tank 241-A W-105, Grab Samples 5A W-95-1, 5A W-95-2 and 5A W-95-3. Three supernate samples exceeded the TOC notification limit (30,000 microg C/g dry weight). Appropriate notifications were made. No immediate notifications were required for any other analyte. The TSAP requested analyses for polychlorinated biphenyls (PCB) for all liquids and centrifuged solid subsamples. The PCB analysis of the liquid samples has been delayed and will be presented in a revision to this document

A Model of Risk Analysis in Analytical Methodology for Biopharmaceutical Quality Control.

Science.gov (United States)

Andrade, Cleyton Lage; Herrera, Miguel Angel De La O; Lemes, Elezer Monte Blanco

2018-01-01

One key quality control parameter for biopharmaceutical products is the analysis of residual cellular DNA. To determine small amounts of DNA (around 100 pg) that may be in a biologically derived drug substance, an analytical method should be sensitive, robust, reliable, and accurate. In principle, three techniques have the ability to measure residual cellular DNA: radioactive dot-blot, a type of hybridization; threshold analysis; and quantitative polymerase chain reaction. Quality risk management is a systematic process for evaluating, controlling, and reporting of risks that may affects method capabilities and supports a scientific and practical approach to decision making. This paper evaluates, by quality risk management, an alternative approach to assessing the performance risks associated with quality control methods used with biopharmaceuticals, using the tool hazard analysis and critical control points. This tool provides the possibility to find the steps in an analytical procedure with higher impact on method performance. By applying these principles to DNA analysis methods, we conclude that the radioactive dot-blot assay has the largest number of critical control points, followed by quantitative polymerase chain reaction, and threshold analysis. From the analysis of hazards (i.e., points of method failure) and the associated method procedure critical control points, we conclude that the analytical methodology with the lowest risk for performance failure for residual cellular DNA testing is quantitative polymerase chain reaction. LAY ABSTRACT: In order to mitigate the risk of adverse events by residual cellular DNA that is not completely cleared from downstream production processes, regulatory agencies have required the industry to guarantee a very low level of DNA in biologically derived pharmaceutical products. The technique historically used was radioactive blot hybridization. However, the technique is a challenging method to implement in a quality

Toward greener analytical techniques for the absolute quantification of peptides in pharmaceutical and biological samples.

Science.gov (United States)

Van Eeckhaut, Ann; Mangelings, Debby

2015-09-10

Peptide-based biopharmaceuticals represent one of the fastest growing classes of new drug molecules. New reaction types included in the synthesis strategies to reduce the rapid metabolism of peptides, along with the availability of new formulation and delivery technologies, resulted in an increased marketing of peptide drug products. In this regard, the development of analytical methods for quantification of peptides in pharmaceutical and biological samples is of utmost importance. From the sample preparation step to their analysis by means of chromatographic or electrophoretic methods, many difficulties should be tackled to analyze them. Recent developments in analytical techniques emphasize more and more on the use of green analytical techniques. This review will discuss the progresses in and challenges observed during green analytical method development for the quantification of peptides in pharmaceutical and biological samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Use of robotic systems for radiochemical sample changing and for analytical sample preparation

International Nuclear Information System (INIS)

Delmastro, J.R.; Hartenstein, S.D.; Wade, M.A.

1989-01-01

Two uses of the Perkin-Elmer (PE) robotic system will be presented. In the first, a PE robot functions as an automatic sample changer for up to five low energy photon spectrometry (LEPS) detectors operated with a Nuclear Data ND 6700 system. The entire system, including the robot, is controlled by an IBM PC-AT using software written in compiled BASIC. Problems associated with the development of the system and modifications to the robot will be presented. In the second, an evaluation study was performed to assess the abilities of the PE robotic system for performing complex analytical sample preparation procedures. For this study, a robotic system based upon the PE robot and auxiliary devices was constructed and programmed to perform the preparation of final product samples (UO 3 ) for accountability and impurity specification analyses. These procedures require sample dissolution, dilution, and liquid-liquid extraction steps. The results of an in-depth evaluation of all system components will be presented

New analytical methodology to reach the actinide determination accuracy ({+-} 2%) required by the OSMOSE program

Energy Technology Data Exchange (ETDEWEB)

Boyer-Deslys, V.; Combaluzier, T.; Dalier, V.; Martin, J.C.; Viallesoubranne, C. [DRCP/SE2A/LAMM, CEA/VALRHO - Marcoule, BP 17171, 30207 Bagnols-sur-Ceze (France); Crozet, M. [LEHA, CEA/VALRHO - Marcoule, BP 17171, 30207 Bagnols-sur-Ceze (France)

2008-07-01

This article describes the analytical procedure optimized by LAMM (Laboratory for Analysis and Materials Methodology) in order to characterize the actinide-doped pellets used in the Osmose (Oscillation in Minerve of isotopes in eupraxis spectra) program (developed for transmutation reactor physics). Osmose aims at providing precise experimental data (absorption cross sections) for heavy nuclides (atomic mass from 232 to 245). This procedure requires the use of the analytical equipment and expertise of the LAMM: TIMS (Thermal Ionization Mass Spectrometer), ICP (Inductively Coupled Plasma) QMS (Quadrupole Mass Spectrometer), SFMS (Sector Field Mass Spectrometer), AES (Atomic Emission Spectrometer), alpha spectrometry and photo-gravimetric analysis. These techniques have met all the specification requirements: extended uncertainties (k=2) below {+-} 2% on the uranium and dopant concentrations, the impurity concentration and the americium-241 concentration.

Selecting Health Care Improvement Projects: A Methodology Integrating Cause-and-Effect Diagram and Analytical Hierarchy Process.

Science.gov (United States)

Testik, Özlem Müge; Shaygan, Amir; Dasdemir, Erdi; Soydan, Guray

It is often vital to identify, prioritize, and select quality improvement projects in a hospital. Yet, a methodology, which utilizes experts' opinions with different points of view, is needed for better decision making. The proposed methodology utilizes the cause-and-effect diagram to identify improvement projects and construct a project hierarchy for a problem. The right improvement projects are then prioritized and selected using a weighting scheme of analytical hierarchy process by aggregating experts' opinions. An approach for collecting data from experts and a graphical display for summarizing the obtained information are also provided. The methodology is implemented for improving a hospital appointment system. The top-ranked 2 major project categories for improvements were identified to be system- and accessibility-related causes (45%) and capacity-related causes (28%), respectively. For each of the major project category, subprojects were then ranked for selecting the improvement needs. The methodology is useful in cases where an aggregate decision based on experts' opinions is expected. Some suggestions for practical implementations are provided.

A GPU code for analytic continuation through a sampling method

Directory of Open Access Journals (Sweden)

Johan Nordström

2016-01-01

Full Text Available We here present a code for performing analytic continuation of fermionic Green’s functions and self-energies as well as bosonic susceptibilities on a graphics processing unit (GPU. The code is based on the sampling method introduced by Mishchenko et al. (2000, and is written for the widely used CUDA platform from NVidia. Detailed scaling tests are presented, for two different GPUs, in order to highlight the advantages of this code with respect to standard CPU computations. Finally, as an example of possible applications, we provide the analytic continuation of model Gaussian functions, as well as more realistic test cases from many-body physics.

A methodology for more efficient tail area sampling with discrete probability distribution

International Nuclear Information System (INIS)

Park, Sang Ryeol; Lee, Byung Ho; Kim, Tae Woon

1988-01-01

Monte Carlo Method is commonly used to observe the overall distribution and to determine the lower or upper bound value in statistical approach when direct analytical calculation is unavailable. However, this method would not be efficient if the tail area of a distribution is concerned. A new method entitled 'Two Step Tail Area Sampling' is developed, which uses the assumption of discrete probability distribution and samples only the tail area without distorting the overall distribution. This method uses two step sampling procedure. First, sampling at points separated by large intervals is done and second, sampling at points separated by small intervals is done with some check points determined at first step sampling. Comparison with Monte Carlo Method shows that the results obtained from the new method converge to analytic value faster than Monte Carlo Method if the numbers of calculation of both methods are the same. This new method is applied to DNBR (Departure from Nucleate Boiling Ratio) prediction problem in design of the pressurized light water nuclear reactor

40 CFR 90.421 - Dilute gaseous exhaust sampling and analytical system description.

Science.gov (United States)

2010-07-01

... gas mixture temperature, measured at a point immediately ahead of the critical flow venturi, must be... analytical system description. (a) General. The exhaust gas sampling system described in this section is... requirements are as follows: (1) This sampling system requires the use of a Positive Displacement Pump—Constant...

Methodological framework, analytical tool and database for the assessment of climate change impacts, adaptation and vulnerability in Denmark

DEFF Research Database (Denmark)

Kaspersen, Per Skougaard; Halsnæs, Kirsten; Gregg, Jay Sterling

. The project is one of seven initiatives proposed by KFT for 2012. The methodology report includes definitions of major concepts, an outline of an analytical structure, a presentation of models and their applicability, and the results of case studies. The work presented in this report draws on intensive...

Nonradioactive Dangerous Waste Landfill sampling and analysis plan and data quality objectives process summary report

International Nuclear Information System (INIS)

Smith, R.C.

1997-08-01

This sampling and analysis plan defines the sampling and analytical activities and associated procedures that will be used to support the Nonradioactive Dangerous Waste Landfill soil-gas investigation. This SAP consists of three sections: this introduction, the field sampling plan, and the quality assurance project plan. The field sampling plan defines the sampling and analytical methodologies to be performed

Recent Trends in Microextraction Techniques Employed in Analytical and Bioanalytical Sample Preparation

Directory of Open Access Journals (Sweden)

Abuzar Kabir

2017-12-01

Full Text Available Sample preparation has been recognized as a major step in the chemical analysis workflow. As such, substantial efforts have been made in recent years to simplify the overall sample preparation process. Major focusses of these efforts have included miniaturization of the extraction device; minimizing/eliminating toxic and hazardous organic solvent consumption; eliminating sample pre-treatment and post-treatment steps; reducing the sample volume requirement; reducing extraction equilibrium time, maximizing extraction efficiency etc. All these improved attributes are congruent with the Green Analytical Chemistry (GAC principles. Classical sample preparation techniques such as solid phase extraction (SPE and liquid-liquid extraction (LLE are being rapidly replaced with emerging miniaturized and environmentally friendly techniques such as Solid Phase Micro Extraction (SPME, Stir bar Sorptive Extraction (SBSE, Micro Extraction by Packed Sorbent (MEPS, Fabric Phase Sorptive Extraction (FPSE, and Dispersive Liquid-Liquid Micro Extraction (DLLME. In addition to the development of many new generic extraction sorbents in recent years, a large number of molecularly imprinted polymers (MIPs created using different template molecules have also enriched the large cache of microextraction sorbents. Application of nanoparticles as high-performance extraction sorbents has undoubtedly elevated the extraction efficiency and method sensitivity of modern chromatographic analyses to a new level. Combining magnetic nanoparticles with many microextraction sorbents has opened up new possibilities to extract target analytes from sample matrices containing high volumes of matrix interferents. The aim of the current review is to critically audit the progress of microextraction techniques in recent years, which has indisputably transformed the analytical chemistry practices, from biological and therapeutic drug monitoring to the environmental field; from foods to phyto

Development and validation of analytical methodology for determination of polycyclic aromatic hydrocarbons (PAHS) in sediments. Assesment of Pedroso Park dam, Santo Andre, SP

International Nuclear Information System (INIS)

Brito, Carlos Fernando de

2009-01-01

The polycyclic aromatic hydrocarbons (PAHs), by being considered persistent contaminants, by their ubiquity in the environment and by the recognition of their genotoxicity, have stimulated research activities in order to determine and evaluate their sources, transport, processing, biological effects and accumulation in compartments of aquatic and terrestrial ecosystems. In this work, the matrix studied was sediment collected at Pedroso Park's dam at Santo Andre, SP. The analytical technique employed was liquid chromatography in reverse phase with a UV/Vis detector. Statistics treatment of the data was established during the process of developing the methodology for which there was reliable results. The steps involved were evaluated using the concept of Validation of Chemical Testing. The parameters selected for the analytical validation were selectivity, linearity, Working Range, Sensitivity, Accuracy, Precision, Limit of Detection, Limit of quantification and robustness. These parameters showed satisfactory results, allowing the application of the methodology, and is a simple method that allows the minimization of contamination and loss of compounds by over-handling. For the PAHs tested were no found positive results, above the limit of detection, in any of the samples collected in the first phase. But, at the second collection, were found small changes mainly acenaphthylene, fluorene and benzo[a]anthracene. Although the area is preserved, it is possible to realize little signs of contamination. (author)

Interpolation and sampling in spaces of analytic functions

CERN Document Server

Seip, Kristian

2004-01-01

The book is about understanding the geometry of interpolating and sampling sequences in classical spaces of analytic functions. The subject can be viewed as arising from three classical topics: Nevanlinna-Pick interpolation, Carleson's interpolation theorem for H^\\infty, and the sampling theorem, also known as the Whittaker-Kotelnikov-Shannon theorem. The book aims at clarifying how certain basic properties of the space at hand are reflected in the geometry of interpolating and sampling sequences. Key words for the geometric descriptions are Carleson measures, Beurling densities, the Nyquist rate, and the Helson-Szegő condition. The book is based on six lectures given by the author at the University of Michigan. This is reflected in the exposition, which is a blend of informal explanations with technical details. The book is essentially self-contained. There is an underlying assumption that the reader has a basic knowledge of complex and functional analysis. Beyond that, the reader should have some familiari...

Preparation of standard hair material and development of analytical methodology

International Nuclear Information System (INIS)

Gangadharan, S.; Walvekar, A.P.; Ali, M.M.; Thantry, S.S.; Verma, R.; Devi, R.

1995-01-01

The concept of the use of human scalp hair as a first level indicator of exposure to inorganic pollutants has been established by us earlier. Efforts towards the preparation of a hair reference material are described. The analytical approaches for the determination of total mercury by cold vapour AAS and INAA and of methylmercury by extraction combined with gas chromatography coupled to an ECD are summarized with results on some of the samples analyzed, including the stability of values over a period of time of storage. (author)

Means of introducing an analyte into liquid sampling atmospheric pressure glow discharge

Science.gov (United States)

Marcus, R. Kenneth; Quarles, Jr., Charles Derrick; Russo, Richard E.; Koppenaal, David W.; Barinaga, Charles J.; Carado, Anthony J.

2017-01-03

A liquid sampling, atmospheric pressure, glow discharge (LS-APGD) device as well as systems that incorporate the device and methods for using the device and systems are described. The LS-APGD includes a hollow capillary for delivering an electrolyte solution to a glow discharge space. The device also includes a counter electrode in the form of a second hollow capillary that can deliver the analyte into the glow discharge space. A voltage across the electrolyte solution and the counter electrode creates the microplasma within the glow discharge space that interacts with the analyte to move it to a higher energy state (vaporization, excitation, and/or ionization of the analyte).

Biofluid infrared spectro-diagnostics: pre-analytical considerations for clinical applications.

Science.gov (United States)

Lovergne, L; Bouzy, P; Untereiner, V; Garnotel, R; Baker, M J; Thiéfin, G; Sockalingum, G D

2016-06-23

Several proof-of-concept studies on the vibrational spectroscopy of biofluids have demonstrated that the methodology has promising potential as a clinical diagnostic tool. However, these studies also show that there is a lack of a standardised protocol in sample handling and preparation prior to spectroscopic analysis. One of the most important sources of analytical errors is the pre-analytical phase. For the technique to be translated into clinics, it is clear that a very strict protocol needs to be established for such biological samples. This study focuses on some of the aspects of the pre-analytical phase in the development of the high-throughput Fourier Transform Infrared (FTIR) spectroscopy of some of the most common biofluids such as serum, plasma and bile. Pre-analytical considerations that can impact either the samples (solvents, anti-coagulants, freeze-thaw cycles…) and/or spectroscopic analysis (sample preparation such as drying, deposit methods, volumes, substrates, operators dependence…) and consequently the quality and the reproducibility of spectral data will be discussed in this report.

Rapid Gamma Screening of Shipments of Analytical Samples to Meet DOT Regulations

International Nuclear Information System (INIS)

Wojtaszek, P.A.; Remington, D.L.; Ideker-Mulligan, V.

2006-01-01

The accelerated closure program at Rocky Flats required the capacity to ship up to 1000 analytical samples per week to off-site commercial laboratories, and to conduct such shipment within 24 hours of sample collection. During a period of near peak activity in the closure project, a regulatory change significantly increased the level of radionuclide data required for shipment of each package. In order to meet these dual challenges, a centralized and streamlined sample management program was developed which channeled analytical samples through a single, high-throughput radiological screening facility. This trailerized facility utilized high purity germanium (HPGe) gamma spectrometers to conduct screening measurements of entire packages of samples at once, greatly increasing throughput compared to previous methods. The In Situ Object Counting System (ISOCS) was employed to calibrate the HPGe systems to accommodate the widely varied sample matrices and packing configurations encountered. Optimum modeling and configuration parameters were determined. Accuracy of the measurements of grouped sample jars was confirmed with blind samples in multiple configurations. Levels of radionuclides not observable by gamma spectroscopy were calculated utilizing a spreadsheet program that can accommodate isotopic ratios for large numbers of different waste streams based upon acceptable knowledge. This program integrated all radionuclide data and output all information required for shipment, including the shipping class of the package. (authors)

The U-tube sampling methodology and real-time analysis of geofluids

International Nuclear Information System (INIS)

Freifeld, Barry; Perkins, Ernie; Underschultz, James; Boreham, Chris

2009-01-01

The U-tube geochemical sampling methodology, an extension of the porous cup technique proposed by Wood (1973), provides minimally contaminated aliquots of multiphase fluids from deep reservoirs and allows for accurate determination of dissolved gas composition. The initial deployment of the U-tube during the Frio Brine Pilot CO 2 storage experiment, Liberty County, Texas, obtained representative samples of brine and supercritical CO 2 from a depth of 1.5 km. A quadrupole mass spectrometer provided real-time analysis of dissolved gas composition. Since the initial demonstration, the U-tube has been deployed for (1) sampling of fluids down gradient of the proposed Yucca Mountain High-Level Waste Repository, Armagosa Valley, Nevada (2) acquiring fluid samples beneath permafrost in Nunuvut Territory, Canada, and (3) at a CO 2 storage demonstration project within a depleted gas reservoir, Otway Basin, Victoria, Australia. The addition of in-line high-pressure pH and EC sensors allows for continuous monitoring of fluid during sample collection. Difficulties have arisen during U-tube sampling, such as blockage of sample lines from naturally occurring waxes or from freezing conditions; however, workarounds such as solvent flushing or heating have been used to address these problems. The U-tube methodology has proven to be robust, and with careful consideration of the constraints and limitations, can provide high quality geochemical samples.

Nuclear analytical techniques and their application to environmental samples

International Nuclear Information System (INIS)

Lieser, K.H.

1986-01-01

A survey is given on nuclear analytical techniques and their application to environmental samples. Measurement of the inherent radioactivity of elements or radionuclides allows determination of natural radioelements (e.g. Ra), man-made radioelements (e.g. Pu) and radionuclides in the environment. Activation analysis, in particular instrumental neutron activation analysis, is a very reliable and sensitive method for determination of a great number of trace elements in environmental samples, because the most abundant main constituents are not activated. Tracer techniques are very useful for studies of the behaviour and of chemical reactions of trace elements and compounds in the environment. Radioactive sources are mainly applied for excitation of characteristic X-rays (X-ray fluorescence analysis). (author)

Results Of Analytical Sample Crosschecks For Next Generation Solvent Extraction Samples Isopar L Concentration And pH

International Nuclear Information System (INIS)

Peters, T.; Fink, S.

2011-01-01

As part of the implementation process for the Next Generation Cesium Extraction Solvent (NGCS), SRNL and F/H Lab performed a series of analytical cross-checks to ensure that the components in the NGCS solvent system do not constitute an undue analytical challenge. For measurement of entrained Isopar(reg s ign) L in aqueous solutions, both labs performed similarly with results more reliable at higher concentrations (near 50 mg/L). Low bias occurred in both labs, as seen previously for comparable blind studies for the baseline solvent system. SRNL recommends consideration to use of Teflon(trademark) caps on all sample containers used for this purpose. For pH measurements, the labs showed reasonable agreement but considerable positive bias for dilute boric acid solutions. SRNL recommends consideration of using an alternate analytical method for qualification of boric acid concentrations.

Performance-based, cost- and time-effective PCB analytical methodology

International Nuclear Information System (INIS)

Alvarado, J. S.

1998-01-01

Laboratory applications for the analysis of PCBs (polychlorinated biphenyls) in environmental matrices such as soil/sediment/sludge and oil/waste oil were evaluated for potential reduction in waste, source reduction, and alternative techniques for final determination. As a consequence, new procedures were studied for solvent substitution, miniaturization of extraction and cleanups, minimization of reagent consumption, reduction of cost per analysis, and reduction of time. These new procedures provide adequate data that meet all the performance requirements for the determination of PCBs. Use of the new procedures reduced costs for all sample preparation techniques. Time and cost were also reduced by combining the new sample preparation procedures with the power of fast gas chromatography. Separation of Aroclor 1254 was achieved in less than 6 min by using DB-1 and SPB-608 columns. With the greatly shortened run times, reproducibility can be tested quickly and consequently with low cost. With performance-based methodology, the applications presented here can be applied now, without waiting for regulatory approval

Analytic continuation of quantum Monte Carlo data. Stochastic sampling method

Energy Technology Data Exchange (ETDEWEB)

Ghanem, Khaldoon; Koch, Erik [Institute for Advanced Simulation, Forschungszentrum Juelich, 52425 Juelich (Germany)

2016-07-01

We apply Bayesian inference to the analytic continuation of quantum Monte Carlo (QMC) data from the imaginary axis to the real axis. Demanding a proper functional Bayesian formulation of any analytic continuation method leads naturally to the stochastic sampling method (StochS) as the Bayesian method with the simplest prior, while it excludes the maximum entropy method and Tikhonov regularization. We present a new efficient algorithm for performing StochS that reduces computational times by orders of magnitude in comparison to earlier StochS methods. We apply the new algorithm to a wide variety of typical test cases: spectral functions and susceptibilities from DMFT and lattice QMC calculations. Results show that StochS performs well and is able to resolve sharp features in the spectrum.

Sample Preparation of Corn Seed Tissue to Prevent Analyte Relocations for Mass Spectrometry Imaging

Science.gov (United States)

Kim, Shin Hye; Kim, Jeongkwon; Lee, Young Jin; Lee, Tae Geol; Yoon, Sohee

2017-08-01

Corn seed tissue sections were prepared by the tape support method using an adhesive tape, and mass spectrometry imaging (MSI) was performed. The effect of heat generated during sample preparation was investigated by time-of-flight secondary mass spectrometry (TOF-SIMS) imaging of corn seed tissue prepared by the tape support and the thaw-mounted methods. Unlike thaw-mounted sample preparation, the tape support method does not cause imaging distortion because of the absence of heat, which can cause migration of the analytes on the sample. By applying the tape-support method, the corn seed tissue was prepared without structural damage and MSI with accurate spatial information of analytes was successfully performed.

Sample Preparation of Corn Seed Tissue to Prevent Analyte Relocations for Mass Spectrometry Imaging.

Science.gov (United States)

Kim, Shin Hye; Kim, Jeongkwon; Lee, Young Jin; Lee, Tae Geol; Yoon, Sohee

2017-08-01

Corn seed tissue sections were prepared by the tape support method using an adhesive tape, and mass spectrometry imaging (MSI) was performed. The effect of heat generated during sample preparation was investigated by time-of-flight secondary mass spectrometry (TOF-SIMS) imaging of corn seed tissue prepared by the tape support and the thaw-mounted methods. Unlike thaw-mounted sample preparation, the tape support method does not cause imaging distortion because of the absence of heat, which can cause migration of the analytes on the sample. By applying the tape-support method, the corn seed tissue was prepared without structural damage and MSI with accurate spatial information of analytes was successfully performed. Graphical Abstract ᅟ.

Recent bibliography on analytical and sampling problems of a PWR primary coolant

International Nuclear Information System (INIS)

Illy, H.

1980-07-01

An extensive bibliography on the problems of analysis and sampling of the primary cooling water of PWRs is presented. The aim was to collect the analytical methods for dissolved gases. The sampling and preparation are also taken into account. last 8-10 years is included. The bibliography is arranged into alphabetical order by topics. The most important topics are as follows: boric acid, gas analysis, hydrogen isotopes, iodine, noble gases, radiation monitoring, sampling and preparation, water chemistry. (R.J.)

MoonDB — A Data System for Analytical Data of Lunar Samples

Science.gov (United States)

Lehnert, K.; Ji, P.; Cai, M.; Evans, C.; Zeigler, R.

2018-04-01

MoonDB is a data system that makes analytical data from the Apollo lunar sample collection and lunar meteorites accessible by synthesizing published and unpublished datasets in a relational database with an online search interface.

Radiochemical methodologies applied to analytical characterization of low and intermediate level wastes from nuclear power plants

Energy Technology Data Exchange (ETDEWEB)

Monteiro, Roberto Pellacani G.; Júnior, Aluísio Souza R.; Kastner, Geraldo F.; Temba, Eliane S.C.; Oliveira, Thiago C. de; Amaral, Ângela M.; Franco, Milton B., E-mail: rpgm@cdtn.br, E-mail: reisas@cdtn.br, E-mail: gfk@cdtn.br, E-mail: esct@cdtn.br, E-mail: tco@cdtn.br, E-mail: ama@cdtn.br, E-mail: francom@cdtn.br [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil)

2017-07-01

The aim of this work is to present radiochemical methodologies developed at CDTN/CNEN in order to answer a program for isotopic inventory of radioactive wastes from Brazilian Nuclear Power Plants. In this program some radionuclides, {sup 3}H, {sup 14}C, {sup 55}Fe, {sup 59}Ni, {sup 63}Ni, {sup 90}Sr, {sup 93}Zr, {sup 94}Nb, {sup 99}Tc, {sup 129}I, {sup 235}U, {sup 238}U, {sup 238}Pu, {sup 239}+{sup 240}Pu, {sup 241}Pu, {sup 242}Pu, {sup 241}Am, {sup 242}Cm e {sup 243}+{sup 244}Cm, were determined in Low Level Wastes (LLW) and Intermediate Level Wastes (ILW) and a protocol of analytical methodologies based on radiochemical separation steps and spectrometric and nuclear techniques was established. (author)

Analytical and computational methodology to assess the over pressures generated by a potential catastrophic failure of a cryogenic pressure vessel

Energy Technology Data Exchange (ETDEWEB)

Zamora, I.; Fradera, J.; Jaskiewicz, F.; Lopez, D.; Hermosa, B.; Aleman, A.; Izquierdo, J.; Buskop, J.

2014-07-01

Idom has participated in the risk evaluation of Safety Important Class (SIC) structures due to over pressures generated by a catastrophic failure of a cryogenic pressure vessel at ITER plant site. The evaluation implements both analytical and computational methodologies achieving consistent and robust results. (Author)

Analytical and computational methodology to assess the over pressures generated by a potential catastrophic failure of a cryogenic pressure vessel

International Nuclear Information System (INIS)

Zamora, I.; Fradera, J.; Jaskiewicz, F.; Lopez, D.; Hermosa, B.; Aleman, A.; Izquierdo, J.; Buskop, J.

2014-01-01

Idom has participated in the risk evaluation of Safety Important Class (SIC) structures due to over pressures generated by a catastrophic failure of a cryogenic pressure vessel at ITER plant site. The evaluation implements both analytical and computational methodologies achieving consistent and robust results. (Author)

Analytical and sampling problems in primary coolant circuits of PWR-type reactors

International Nuclear Information System (INIS)

Illy, H.

1980-10-01

Details of recent analytical methods on the analysis and sampling of a PWR primary coolant are given in the order as follows: sampling and preparation; analysis of the gases dissolved in the water; monitoring of radiating substances; checking of boric acid concentration which controls the reactivity. The bibliography of this work and directions for its use are published in a separate report: KFKI-80-48 (1980). (author)

Collaborative Visual Analytics: A Health Analytics Approach to Injury Prevention.

Science.gov (United States)

Al-Hajj, Samar; Fisher, Brian; Smith, Jennifer; Pike, Ian

2017-09-12

Background : Accurate understanding of complex health data is critical in order to deal with wicked health problems and make timely decisions. Wicked problems refer to ill-structured and dynamic problems that combine multidimensional elements, which often preclude the conventional problem solving approach. This pilot study introduces visual analytics (VA) methods to multi-stakeholder decision-making sessions about child injury prevention; Methods : Inspired by the Delphi method, we introduced a novel methodology-group analytics (GA). GA was pilot-tested to evaluate the impact of collaborative visual analytics on facilitating problem solving and supporting decision-making. We conducted two GA sessions. Collected data included stakeholders' observations, audio and video recordings, questionnaires, and follow up interviews. The GA sessions were analyzed using the Joint Activity Theory protocol analysis methods; Results : The GA methodology triggered the emergence of ' common g round ' among stakeholders. This common ground evolved throughout the sessions to enhance stakeholders' verbal and non-verbal communication, as well as coordination of joint activities and ultimately collaboration on problem solving and decision-making; Conclusion s : Understanding complex health data is necessary for informed decisions. Equally important, in this case, is the use of the group analytics methodology to achieve ' common ground' among diverse stakeholders about health data and their implications.

An analytical examination of distortions in power spectra due to sampling errors

International Nuclear Information System (INIS)

Njau, E.C.

1982-06-01

Distortions introduced into spectral energy densities of sinusoid signals as well as those of more complex signals through different forms of errors in signal sampling are developed and shown analytically. The approach we have adopted in doing this involves, firstly, developing for each type of signal and for the corresponding form of sampling errors an analytical expression that gives the faulty digitization process involved in terms of the features of the particular signal. Secondly, we take advantage of a method described elsewhere [IC/82/44] to relate, as much as possible, the true spectral energy density of the signal and the corresponding spectral energy density of the faulty digitization process. Thirdly, we then develop expressions which reveal the distortions that are formed in the directly computed spectral energy density of the digitized signal. It is evident from the formulations developed herein that the types of sampling errors taken into consideration may create false peaks and other distortions that are of non-negligible concern in computed power spectra. (author)

Develop of analytic method for the determination of vitamin D3 in multivitaminics and minerals using chromatography it liquidates of high efficiency in normal phase with ultraviolet detection

International Nuclear Information System (INIS)

Solis Barrantes, J. A.

1999-01-01

The good chromatography conditions settled down for the determination vitamin D 3 in multivitaminic samples by means of the analytic technique of chromatography it liquidates of high efficiency (HPLC) in normal phase, with ultraviolet detection to 265 nm. The best conditions in the proposed methodology settled down and the variables of analytic acting were validated, for the analytic quantification of vitamin D 3 in International units. The applicability of the methodology was demonstrated in the vitamin determination D 3 in multivitaminis samples in pill form [es

Methodological and Analytical Dilemmas in Autoethnographic Research

Directory of Open Access Journals (Sweden)

Elena Maydell

2010-01-01

Full Text Available This article presents an argument on the application of theoretical and methodological frameworks to the study of identity from an autoethnographic perspective. In order to guide the analysis process, the author employed social constructionism as the main theoretical foundation, whereas thematic analysis and positioning theory were deployed as the methodological frameworks. Further, in the process of using ethnographic methods to study the identity of Russian immigrants to New Zealand, the author found herself also needing to use autoethnography to interrogate and understand her own journey. The insider/outsider position of the author who belongs to the same minority group became the most vital tool in her identity construction. In this regard, it is impossible to engage fully with the autoethnographic research practice without understanding the impact of others on identity construction of self, and a strong theoretical and methodological scholarship can provide a valuable foundation for this process.

Methodological quality of meta-analyses on treatments for chronic obstructive pulmonary disease: a cross-sectional study using the AMSTAR (Assessing the Methodological Quality of Systematic Reviews) tool.

Science.gov (United States)

Ho, Robin S T; Wu, Xinyin; Yuan, Jinqiu; Liu, Siya; Lai, Xin; Wong, Samuel Y S; Chung, Vincent C H

2015-01-08

Meta-analysis (MA) of randomised trials is considered to be one of the best approaches for summarising high-quality evidence on the efficacy and safety of treatments. However, methodological flaws in MAs can reduce the validity of conclusions, subsequently impairing the quality of decision making. To assess the methodological quality of MAs on COPD treatments. A cross-sectional study on MAs of COPD trials. MAs published during 2000-2013 were sampled from the Cochrane Database of Systematic Reviews and Database of Abstracts of Reviews of Effect. Methodological quality was assessed using the validated AMSTAR (Assessing the Methodological Quality of Systematic Reviews) tool. Seventy-nine MAs were sampled. Only 18% considered the scientific quality of primary studies when formulating conclusions and 49% used appropriate meta-analytic methods to combine findings. The problems were particularly acute among MAs on pharmacological treatments. In 48% of MAs the authors did not report conflict of interest. Fifty-eight percent reported harmful effects of treatment. Publication bias was not assessed in 65% of MAs, and only 10% had searched non-English databases. The methodological quality of the included MAs was disappointing. Consideration of scientific quality when formulating conclusions should be made explicit. Future MAs should improve on reporting conflict of interest and harm, assessment of publication bias, prevention of language bias and use of appropriate meta-analytic methods.

State of the art of environmentally friendly sample preparation approaches for determination of PBDEs and metabolites in environmental and biological samples: A critical review.

Science.gov (United States)

Berton, Paula; Lana, Nerina B; Ríos, Juan M; García-Reyes, Juan F; Altamirano, Jorgelina C

2016-01-28

Green chemistry principles for developing methodologies have gained attention in analytical chemistry in recent decades. A growing number of analytical techniques have been proposed for determination of organic persistent pollutants in environmental and biological samples. In this light, the current review aims to present state-of-the-art sample preparation approaches based on green analytical principles proposed for the determination of polybrominated diphenyl ethers (PBDEs) and metabolites (OH-PBDEs and MeO-PBDEs) in environmental and biological samples. Approaches to lower the solvent consumption and accelerate the extraction, such as pressurized liquid extraction, microwave-assisted extraction, and ultrasound-assisted extraction, are discussed in this review. Special attention is paid to miniaturized sample preparation methodologies and strategies proposed to reduce organic solvent consumption. Additionally, extraction techniques based on alternative solvents (surfactants, supercritical fluids, or ionic liquids) are also commented in this work, even though these are scarcely used for determination of PBDEs. In addition to liquid-based extraction techniques, solid-based analytical techniques are also addressed. The development of greener, faster and simpler sample preparation approaches has increased in recent years (2003-2013). Among green extraction techniques, those based on the liquid phase predominate over those based on the solid phase (71% vs. 29%, respectively). For solid samples, solvent assisted extraction techniques are preferred for leaching of PBDEs, and liquid phase microextraction techniques are mostly used for liquid samples. Likewise, green characteristics of the instrumental analysis used after the extraction and clean-up steps are briefly discussed. Copyright © 2015 Elsevier B.V. All rights reserved.

Development of an analytical methodology for the determination of the antiparasitic drug toltrazuril and its two metabolites in surface water, soil and animal manure

DEFF Research Database (Denmark)

Olsen, Jesper; Björklund, Erland; Krogh, Kristine A

2012-01-01

This paper presents the development, optimization and validation of a LC-MS/MS methodology to determine the antiparasitic veterinary drug toltrazuril and its two main metabolites, toltrazuril sulfoxide and toltrazuril sulfone, in environmental surface water, soil and animal manure. Using solid...... phase extraction and selective pressurized liquid extraction with integrated clean-up, the analytical method allows for the determination of these compounds down to 0.06-0.13 ng L(-1) in water, 0.01-0.03 ng g(-1)dw in soil and 0.22-0.51 ng g(-1) dw in manure. The deuterated analog of toltrazuril...... was used as internal standard, and ensured method accuracy in the range 96-123% for water and 77-110% for soil samples. The developed method can also be applied to simultaneously determine steroid hormones in the solid samples. The antiparasitic drug and its metabolites were found in manure and soil up...

Computerized Analytical Data Management System and Automated Analytical Sample Transfer System at the COGEMA Reprocessing Plants in La Hague

International Nuclear Information System (INIS)

Flament, T.; Goasmat, F.; Poilane, F.

2002-01-01

Managing the operation of large commercial spent nuclear fuel reprocessing plants, such as UP3 and UP2-800 in La Hague, France, requires an extensive analytical program and the shortest possible analysis response times. COGEMA, together with its engineering subsidiary SGN, decided to build high-performance laboratories to support operations in its plants. These laboratories feature automated equipment, safe environments for operators, and short response times, all in centralized installations. Implementation of a computerized analytical data management system and a fully automated pneumatic system for the transfer of radioactive samples was a key factor contributing to the successful operation of the laboratories and plants

Automated Sample Preparation for Radiogenic and Non-Traditional Metal Isotopes: Removing an Analytical Barrier for High Sample Throughput

Science.gov (United States)

Field, M. Paul; Romaniello, Stephen; Gordon, Gwyneth W.; Anbar, Ariel D.; Herrmann, Achim; Martinez-Boti, Miguel A.; Anagnostou, Eleni; Foster, Gavin L.

2014-05-01

MC-ICP-MS has dramatically improved the analytical throughput for high-precision radiogenic and non-traditional isotope ratio measurements, compared to TIMS. The generation of large data sets, however, remains hampered by tedious manual drip chromatography required for sample purification. A new, automated chromatography system reduces the laboratory bottle neck and expands the utility of high-precision isotope analyses in applications where large data sets are required: geochemistry, forensic anthropology, nuclear forensics, medical research and food authentication. We have developed protocols to automate ion exchange purification for several isotopic systems (B, Ca, Fe, Cu, Zn, Sr, Cd, Pb and U) using the new prepFAST-MC™ (ESI, Nebraska, Omaha). The system is not only inert (all-flouropolymer flow paths), but is also very flexible and can easily facilitate different resins, samples, and reagent types. When programmed, precise and accurate user defined volumes and flow rates are implemented to automatically load samples, wash the column, condition the column and elute fractions. Unattended, the automated, low-pressure ion exchange chromatography system can process up to 60 samples overnight. Excellent reproducibility, reliability, recovery, with low blank and carry over for samples in a variety of different matrices, have been demonstrated to give accurate and precise isotopic ratios within analytical error for several isotopic systems (B, Ca, Fe, Cu, Zn, Sr, Cd, Pb and U). This illustrates the potential of the new prepFAST-MC™ (ESI, Nebraska, Omaha) as a powerful tool in radiogenic and non-traditional isotope research.

Sample diagnosis using indicator elements and non-analyte signals for inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Antler, Margaret; Ying Hai; Burns, David H.; Salin, Eric D.

2003-01-01

A sample diagnosis procedure that uses both non-analyte and analyte signals to estimate matrix effects in inductively coupled plasma-mass spectrometry is presented. Non-analyte signals are those of background species in the plasma (e.g. N + , ArO + ), and changes in these signals can indicate changes in plasma conditions. Matrix effects of Al, Ba, Cs, K and Na on 19 non-analyte signals and 15 element signals were monitored. Multiple linear regression was used to build the prediction models, using a genetic algorithm for objective feature selection. Non-analyte elemental signals and non-analyte signals were compared for diagnosing matrix effects, and both were found to be suitable for estimating matrix effects. Individual analyte matrix effect estimation was compared with the overall matrix effect prediction, and models used to diagnose overall matrix effects were more accurate than individual analyte models. In previous work [Spectrochim. Acta Part B 57 (2002) 277], we tested models for analytical decision making. The current models were tested in the same way, and were able to successfully diagnose matrix effects with at least an 80% success rate

Analytical artefacts in the speciation of arsenic in clinical samples

International Nuclear Information System (INIS)

Slejkovec, Zdenka; Falnoga, Ingrid; Goessler, Walter; Elteren, Johannes T. van; Raml, Reingard; Podgornik, Helena; Cernelc, Peter

2008-01-01

Urine and blood samples of cancer patients, treated with high doses of arsenic trioxide were analysed for arsenic species using HPLC-HGAFS and, in some cases, HPLC-ICPMS. Total arsenic was determined with either flow injection-HGAFS in urine or radiochemical neutron activation analysis in blood fractions (in serum/plasma, blood cells). The total arsenic concentrations (during prolonged, daily/weekly arsenic trioxide therapy) were in the μg mL -1 range for urine and in the ng g -1 range for blood fractions. The main arsenic species found in urine were As(III), MA and DMA and in blood As(V), MA and DMA. With proper sample preparation and storage of urine (no preservation agents/storage in liquid nitrogen) no analytical artefacts were observed and absence of significant amounts of alleged trivalent metabolites was proven. On the contrary, in blood samples a certain amount of arsenic can get lost in the speciation procedure what was especially noticeable for the blood cells although also plasma/serum gave rise to some disappearance of arsenic. The latter losses may be attributed to precipitation of As(III)-containing proteins/peptides during the methanol/water extraction procedure whereas the former losses were due to loss of specific As(III)-complexing proteins/peptides (e.g. cysteine, metallothionein, reduced GSH, ferritin) on the column (Hamilton PRP-X100) during the separation procedure. Contemporary analytical protocols are not able to completely avoid artefacts due to losses from the sampling to the detection stage so that it is recommended to be careful with the explanation of results, particularly regarding metabolic and pharmacokinetic interpretations, and always aim to compare the sum of species with the total arsenic concentration determined independently

Accounting for methodological, structural, and parameter uncertainty in decision-analytic models: a practical guide.

Science.gov (United States)

Bilcke, Joke; Beutels, Philippe; Brisson, Marc; Jit, Mark

2011-01-01

Accounting for uncertainty is now a standard part of decision-analytic modeling and is recommended by many health technology agencies and published guidelines. However, the scope of such analyses is often limited, even though techniques have been developed for presenting the effects of methodological, structural, and parameter uncertainty on model results. To help bring these techniques into mainstream use, the authors present a step-by-step guide that offers an integrated approach to account for different kinds of uncertainty in the same model, along with a checklist for assessing the way in which uncertainty has been incorporated. The guide also addresses special situations such as when a source of uncertainty is difficult to parameterize, resources are limited for an ideal exploration of uncertainty, or evidence to inform the model is not available or not reliable. for identifying the sources of uncertainty that influence results most are also described. Besides guiding analysts, the guide and checklist may be useful to decision makers who need to assess how well uncertainty has been accounted for in a decision-analytic model before using the results to make a decision.

Development of a novel methodology for indoor emission source identification

DEFF Research Database (Denmark)

Han, K.H.; Zhang, J.S.; Knudsen, H.N.

2011-01-01

The objective of this study was to develop and evaluate a methodology to identify individual sources of emissions based on the measurements of mixed air samples and the emission signatures of individual materials previously determined by Proton Transfer Reaction-Mass Spectrometry (PTR-MS), an on......-line analytical device. The methodology based on signal processing principles was developed by employing the method of multiple regression least squares (MRLS) and a normalization technique. Samples of nine typical building materials were tested individually and in combination, including carpet, ceiling material...... experiments and investigation are needed for cases where the relative emission rates among different compounds may change over a long-term period....

Analytical Issues on the Determination of Carotenoids in Microalgae by Liquid Chromatography with Diode Array Detector

International Nuclear Information System (INIS)

Garcia, S.; Perez, R. M.

2012-01-01

A preliminary study of literature review on the determination of carotenoids in microalgae samples by HPLC with diode array detector is presented. Main objective has been focused to compile data from literature and based on the main aspects of the analytical methodology used in the determination of these compounds. The work is structured as follows and affecting major analytical difficulties: Procurement and commercial availability of standard solutions. Stage of sample treatment. Chromatographic analysis. (Author) 19 refs.

Paper Capillary Enables Effective Sampling for Microfluidic Paper Analytical Devices.

Science.gov (United States)

Shangguan, Jin-Wen; Liu, Yu; Wang, Sha; Hou, Yun-Xuan; Xu, Bi-Yi; Xu, Jing-Juan; Chen, Hong-Yuan

2018-06-06

Paper capillary is introduced to enable effective sampling on microfluidic paper analytical devices. By coupling mac-roscale capillary force of paper capillary and microscale capillary forces of native paper, fluid transport can be flexibly tailored with proper design. Subsequently, a hybrid-fluid-mode paper capillary device was proposed, which enables fast and reliable sampling in an arrayed form, with less surface adsorption and bias for different components. The resulting device thus well supports high throughput, quantitative, and repeatable assays all by hands operation. With all these merits, multiplex analysis of ions, proteins, and microbe have all been realized on this platform, which has paved the way to level-up analysis on μPADs.

Stability of Circulating Blood-Based MicroRNAs - Pre-Analytic Methodological Considerations.

Directory of Open Access Journals (Sweden)

Charlotte Glinge

Full Text Available The potential of microRNAs (miRNA as non-invasive diagnostic, prognostic, and predictive biomarkers, as well as therapeutic targets, has recently been recognized. Previous studies have highlighted the importance of consistency in the methodology used, but to our knowledge, no study has described the methodology of sample preparation and storage systematically with respect to miRNAs as blood biomarkers. The aim of this study was to investigate the stability of miRNAs in blood under various relevant clinical and research conditions: different collection tubes, storage at different temperatures, physical disturbance, as well as serial freeze-thaw cycles.Blood samples were collected from 12 healthy donors into different collection tubes containing anticoagulants, including EDTA, citrate and lithium-heparin, as well as into serum collection tubes. MiRNA stability was evaluated by measuring expression changes of miR-1, miR-21 and miR-29b at different conditions: varying processing time of whole blood (up to 72 hours (h, long-term storage (9 months at -80°C, physical disturbance (1 and 8 h, as well as in a series of freeze/thaw cycles (1 and 4 times.Different collection tubes revealed comparable concentrations of miR-1, miR-21 and miR-29b. Tubes with lithium-heparin were found unsuitable for miRNA quantification. MiRNA levels were stable for at least 24 h at room temperature in whole blood, while separated fractions did show alterations within 24 h. There were significant changes in the miR-21 and miR-29b levels after 72 h incubation of whole blood at room temperature (p<0.01 for both. Both miR-1 and miR-21 showed decreased levels after physical disturbance for 8 h in separated plasma and miR-1 in serum whole blood, while after 1 h of disturbance no changes were observed. Storage of samples at -80°C extended the miRNA stability remarkably, however, miRNA levels in long-term stored (9 months whole blood samples were significantly changed, which is in

Evaluation methodology for comparing memory and communication of analytic processes in visual analytics

Energy Technology Data Exchange (ETDEWEB)

Ragan, Eric D [ORNL; Goodall, John R [ORNL

2014-01-01

Provenance tools can help capture and represent the history of analytic processes. In addition to supporting analytic performance, provenance tools can be used to support memory of the process and communication of the steps to others. Objective evaluation methods are needed to evaluate how well provenance tools support analyst s memory and communication of analytic processes. In this paper, we present several methods for the evaluation of process memory, and we discuss the advantages and limitations of each. We discuss methods for determining a baseline process for comparison, and we describe various methods that can be used to elicit process recall, step ordering, and time estimations. Additionally, we discuss methods for conducting quantitative and qualitative analyses of process memory. By organizing possible memory evaluation methods and providing a meta-analysis of the potential benefits and drawbacks of different approaches, this paper can inform study design and encourage objective evaluation of process memory and communication.

Time and temperature dependent analytical stability of dry-collected Evalyn HPV self-sampling brush for cervical cancer screening

DEFF Research Database (Denmark)

Ejegod, Ditte Møller; Pedersen, Helle; Alzua, Garazi Peña

2018-01-01

As a new initiative, HPV self-sampling to non-attenders using the dry Evalyn self-sampling brush is offered in the Capital Region of Denmark. The use of a dry brush is largely uncharted territory in terms of analytical stability. In this study we aim to provide evidence on the analytical quality...

Abstracts book of 4. Poznan Analytical Seminar on Modern Methods of Sample Preparation and Trace Amounts Determination of Elements

International Nuclear Information System (INIS)

1995-01-01

The 4. Poznan Analytical Seminar on Modern Methods of Sample Preparation and Trace Amounts Determination of Elements has been held in Poznan 27-28 April 1995. The new versions of analytical methods have been presented for quantitative determination of trace elements in biological, environmental and geological materials. Also the number of special techniques for sample preparation enables achievement the best precision of analytical results have been shown and discussed

Statistics and sampling in transuranic studies

International Nuclear Information System (INIS)

Eberhardt, L.L.; Gilbert, R.O.

1980-01-01

The existing data on transuranics in the environment exhibit a remarkably high variability from sample to sample (coefficients of variation of 100% or greater). This chapter stresses the necessity of adequate sample size and suggests various ways to increase sampling efficiency. Objectives in sampling are regarded as being of great importance in making decisions as to sampling methodology. Four different classes of sampling methods are described: (1) descriptive sampling, (2) sampling for spatial pattern, (3) analytical sampling, and (4) sampling for modeling. A number of research needs are identified in the various sampling categories along with several problems that appear to be common to two or more such areas

New analytical methodology for analysing S(IV) species at low pH solutions by one stage titration method (bichromatometry) with a clear colour change. Could potentially replace the state-of-art-method iodometry at low pH analysis due higher accuracy.

Science.gov (United States)

Santasalo-Aarnio, Annukka; Galfi, Istvan; Virtanen, Jorma; Gasik, Michael M

2017-01-01

A new, faster and more reliable analytical methodology for S(IV) species analysis at low pH solutions by bichromatometry is proposed. For decades the state of the art methodology has been iodometry that is still well justified method for neutral solutions, thus at low pH media possess various side reactions increasing inaccuracy. In contrast, the new methodology has no side reactions at low pH media, requires only one titration step and provides a clear color change if S(IV) species are present in the solution. The method is validated using model solutions with known concentrations and applied to analyses of gaseous SO2 from purged solution in low pH media samples. The results indicate that bichromatometry can accurately analyze SO2 from liquid samples having pH even below 0 relevant to metallurgical industrial processes.

Analytical tools and methodologies for evaluation of residual life of contacting pressure tubes in the early generation of Indian PHWRs

International Nuclear Information System (INIS)

Sinha, S.K.; Madhusoodanan, K.; Rupani, B.B.; Sinha, R.K.

2002-01-01

In-service life of a contacting Zircaloy-2 pressure tube (PT) in the earlier generation of Indian PHWRs, is limited mainly due to the accelerated hydrogen pick-up and nucleation and growth of hydride blister(s) at the cold spot(s) formed on outside surface of pressure tube as a result of its contact with the calandria tube (CT). The activities involving development of the analytical models for simulating the degradation mechanisms leading to PT-CT contact and the methodologies for the revaluation of their safe life under such condition form the important part of our extensive programme for the life management of contacting pressure tubes. Since after the PT-CT contact, rate of hydrogen pick-up and nucleation and growth of hydride blisters govern the safe residual life of the pressure tube, two analytical models (a) hydrogen pick-up model ('HYCON') and (b) model for the nucleation and growth of hydride blister at the contact spot ('BLIST -2D') have been developed in-house to estimate the extent of degradation caused by them. Along with them, a methodology for evaluation of safe residual life has also been formulated for evaluating the safe residual life of the contacting channels. This paper gives the brief description of the models and the methodologies relevant for the contacting Zircaloy-2 pressure tubes. (author)

Understanding User-Web Interactions via Web Analytics

CERN Document Server

Jansen, Bernard J

2009-01-01

This lecture presents an overview of the Web analytics process, with a focus on providing insight and actionable outcomes from collecting and analyzing Internet data. The lecture first provides an overview of Web analytics, providing in essence, a condensed version of the entire lecture. The lecture then outlines the theoretical and methodological foundations of Web analytics in order to make obvious the strengths and shortcomings of Web analytics as an approach. These foundational elements include the psychological basis in behaviorism and methodological underpinning of trace data as an empir

Negative dielectrophoresis spectroscopy for rare analyte quantification in biological samples

Science.gov (United States)

Kirmani, Syed Abdul Mannan; Gudagunti, Fleming Dackson; Velmanickam, Logeeshan; Nawarathna, Dharmakeerthi; Lima, Ivan T., Jr.

2017-03-01

We propose the use of negative dielectrophoresis (DEP) spectroscopy as a technique to improve the detection limit of rare analytes in biological samples. We observe a significant dependence of the negative DEP force on functionalized polystyrene beads at the edges of interdigitated electrodes with respect to the frequency of the electric field. We measured this velocity of repulsion for 0% and 0.8% conjugation of avidin with biotin functionalized polystyrene beads with our automated software through real-time image processing that monitors the Rayleigh scattering from the beads. A significant difference in the velocity of the beads was observed in the presence of as little as 80 molecules of avidin per biotin functionalized bead. This technology can be applied in the detection and quantification of rare analytes that can be useful in the diagnosis and the treatment of diseases, such as cancer and myocardial infarction, with the use of polystyrene beads functionalized with antibodies for the target biomarkers.

Review of Analytes of Concern and Sample Methods for Closure of DOE High Level Waste Storage Tanks

International Nuclear Information System (INIS)

Thomas, T.R.

2002-01-01

Sampling residual waste after tank cleaning and analysis for analytes of concern to support closure and cleaning targets of large underground tanks used for storage of legacy high level radioactive waste (HLW) at Department of Energy (DOE) sites has been underway since about 1995. The DOE Tanks Focus Area (TFA) has been working with DOE tank sites to develop new sampling plans, and sampling methods for assessment of residual waste inventories. This paper discusses regulatory analytes of concern, sampling plans, and sampling methods that support closure and cleaning target activities for large storage tanks at the Hanford Site, the Savannah River Site (SRS), the Idaho National Engineering and Environmental Laboratory (INEEL), and the West Valley Demonstration Project (WVDP)

Municipal solid waste composition: Sampling methodology, statistical analyses, and case study evaluation

DEFF Research Database (Denmark)

Edjabou, Vincent Maklawe Essonanawe; Jensen, Morten Bang; Götze, Ramona

2015-01-01

Sound waste management and optimisation of resource recovery require reliable data on solid waste generation and composition. In the absence of standardised and commonly accepted waste characterisation methodologies, various approaches have been reported in literature. This limits both...... comparability and applicability of the results. In this study, a waste sampling and sorting methodology for efficient and statistically robust characterisation of solid waste was introduced. The methodology was applied to residual waste collected from 1442 households distributed among 10 individual sub......-areas in three Danish municipalities (both single and multi-family house areas). In total 17 tonnes of waste were sorted into 10-50 waste fractions, organised according to a three-level (tiered approach) facilitating,comparison of the waste data between individual sub-areas with different fractionation (waste...

Characterization of carbon nanotubes and analytical methods for their determination in environmental and biological samples: A review

Energy Technology Data Exchange (ETDEWEB)

Herrero-Latorre, C., E-mail: carlos.herrero@usc.es; Álvarez-Méndez, J.; Barciela-García, J.; García-Martín, S.; Peña-Crecente, R.M.

2015-01-01

Highlights: • Analytical techniques for characterization of CNTs: classification, description and examples. • Determination methods for CNTs in biological and environmental samples. • Future trends and perspectives for characterization and determination of CNTs. - Abstract: In the present paper, a critical overview of the most commonly used techniques for the characterization and the determination of carbon nanotubes (CNTs) is given on the basis of 170 references (2000–2014). The analytical techniques used for CNT characterization (including microscopic and diffraction, spectroscopic, thermal and separation techniques) are classified, described, and illustrated with applied examples. Furthermore, the performance of sampling procedures as well as the available methods for the determination of CNTs in real biological and environmental samples are reviewed and discussed according to their analytical characteristics. In addition, future trends and perspectives in this field of work are critically presented.

Improved analytical sensitivity for uranium and plutonium in environmental samples: Cavity ion source thermal ionization mass spectrometry

International Nuclear Information System (INIS)

Ingeneri, Kristofer; Riciputi, L.

2001-01-01

Following successful field trials, environmental sampling has played a central role as a routine part of safeguards inspections since early 1996 to verify declared and to detect undeclared activity. The environmental sampling program has brought a new series of analytical challenges, and driven a need for advances in verification technology. Environmental swipe samples are often extremely low in concentration of analyte (ng level or lower), yet the need to analyze these samples accurately and precisely is vital, particularly for the detection of undeclared nuclear activities. Thermal ionization mass spectrometry (TIMS) is the standard method of determining isotope ratios of uranium and plutonium in the environmental sampling program. TIMS analysis typically employs 1-3 filaments to vaporize and ionize the sample, and the ions are mass separated and analyzed using magnetic sector instruments due to their high mass resolution and high ion transmission. However, the ionization efficiency (the ratio of material present to material actually detected) of uranium using a standard TIMS instrument is low (0.2%), even under the best conditions. Increasing ionization efficiency by even a small amount would have a dramatic impact for safeguards applications, allowing both improvements in analytical precision and a significant decrease in the amount of uranium and plutonium required for analysis, increasing the sensitivity of environmental sampling

Atmospheric Deposition: Sampling Procedures, Analytical Methods, and Main Recent Findings from the Scientific Literature

Directory of Open Access Journals (Sweden)

M. Amodio

2014-01-01

Full Text Available The atmosphere is a carrier on which some natural and anthropogenic organic and inorganic chemicals are transported, and the wet and dry deposition events are the most important processes that remove those chemicals, depositing it on soil and water. A wide variety of different collectors were tested to evaluate site-specificity, seasonality and daily variability of settleable particle concentrations. Deposition fluxes of POPs showed spatial and seasonal variations, diagnostic ratios of PAHs on deposited particles, allowed the discrimination between pyrolytic or petrogenic sources. Congener pattern analysis and bulk deposition fluxes in rural sites confirmed long-range atmospheric transport of PCDDs/Fs. More and more sophisticated and newly designed deposition samplers have being used for characterization of deposited mercury, demonstrating the importance of rain scavenging and the relatively higher magnitude of Hg deposition from Chinese anthropogenic sources. Recently biological monitors demonstrated that PAH concentrations in lichens were comparable with concentrations measured in a conventional active sampler in an outdoor environment. In this review the authors explore the methodological approaches used for the assessment of atmospheric deposition, from the analysis of the sampling methods, the analytical procedures for chemical characterization of pollutants and the main results from the scientific literature.

Review of robust measurement of phosphorus in river water: sampling, storage, fractionation and sensitivity

Directory of Open Access Journals (Sweden)

H. P. Jarvie

2002-01-01

Full Text Available This paper reviews current knowledge on sampling, storage and analysis of phosphorus (P in river waters. Potential sensitivity of rivers with different physical, chemical and biological characteristics (trophic status, turbidity, flow regime, matrix chemistry is examined in terms of errors associated with sampling, sample preparation, storage, contamination, interference and analytical errors. Key issues identified include: The need to tailor analytical reagents and concentrations to take into account the characteristics of the sample matrix. The effects of matrix interference on the colorimetric analysis. The influence of variable rates of phospho-molybdenum blue colour formation. The differing responses of river waters to physical and chemical conditions of storage. The higher sensitivities of samples with low P concentrations to storage and analytical errors. Given high variability of river water characteristics in space and time, no single standardised methodology for sampling, storage and analysis of P in rivers can be offered. ‘Good Practice’ guidelines are suggested, which recommend that protocols for sampling, storage and analysis of river water for P is based on thorough site-specific method testing and assessment of P stability on storage. For wider sampling programmes at the regional/national scale where intensive site-specific method and stability testing are not feasible, ‘Precautionary Practice’ guidelines are suggested. The study highlights key areas requiring further investigation for improving methodological rigour. Keywords: phosphorus, orthophosphate, soluble reactive, particulate, colorimetry, stability, sensitivity, analytical error, storage, sampling, filtration, preservative, fractionation, digestion

Quality assesment for the analysis of PCDDs/PCDFs in individual human serum samples

Energy Technology Data Exchange (ETDEWEB)

Perez, F [IIQAB-CSIC, Barcelona (Spain). Dept. of Ecotechnologies, Lab. of Dioxins; Abad, E; Llerena, J J; Caixach, J; Rivera, J

2004-09-15

The aim of this work was to optimise a relevant methodology for the ultratrace analysis of PCDDs/PCDFs in individual human serum samples. In order to carry out the study, different strategies including the elaboration of quality control samples, parallel sample analysis, control blanks and a number of quality assurance measures were implemented as analytical current practices. Some of the main drawbacks in the analysis of PCDDs/PCDFs in these kind of samples come from two conflicting aspects: the small sample size and the low levels expected to be found. Taking this into account, an unavoidable compromise between the sample amount and the minimum analytical requirements, mainly the detection limit (LOD), is mandatory. To reach this goal C{sub 18} solid phase extraction was used to remove the analytes from the matrix. Clean up was performed by solid-liquid adsorption chromatography using a variety of adsorbents. Instrumental analysis was achieved by high-resolution gas chromatography coupled to high-resolution mass spectrometry (HRGC/HRMS). Finally, the optimised methodology was applied to evaluate the potential impact in general population living in the surroundings of an obsolete municipal waste incinerator plant (MWI). Thus, more than 400 individuals serum samples potentially exposed to the emission of the incinerator and people not exposed were considered in this study.

Biomass Thermogravimetric Analysis: Uncertainty Determination Methodology and Sampling Maps Generation

Science.gov (United States)

Pazó, Jose A.; Granada, Enrique; Saavedra, Ángeles; Eguía, Pablo; Collazo, Joaquín

2010-01-01

The objective of this study was to develop a methodology for the determination of the maximum sampling error and confidence intervals of thermal properties obtained from thermogravimetric analysis (TG), including moisture, volatile matter, fixed carbon and ash content. The sampling procedure of the TG analysis was of particular interest and was conducted with care. The results of the present study were compared to those of a prompt analysis, and a correlation between the mean values and maximum sampling errors of the methods were not observed. In general, low and acceptable levels of uncertainty and error were obtained, demonstrating that the properties evaluated by TG analysis were representative of the overall fuel composition. The accurate determination of the thermal properties of biomass with precise confidence intervals is of particular interest in energetic biomass applications. PMID:20717532

Analytical Parameters of an Amperometric Glucose Biosensor for Fast Analysis in Food Samples.

Science.gov (United States)

Artigues, Margalida; Abellà, Jordi; Colominas, Sergi

2017-11-14

Amperometric biosensors based on the use of glucose oxidase (GOx) are able to combine the robustness of electrochemical techniques with the specificity of biological recognition processes. However, very little information can be found in literature about the fundamental analytical parameters of these sensors. In this work, the analytical behavior of an amperometric biosensor based on the immobilization of GOx using a hydrogel (Chitosan) onto highly ordered titanium dioxide nanotube arrays (TiO₂NTAs) has been evaluated. The GOx-Chitosan/TiO₂NTAs biosensor showed a sensitivity of 5.46 μA·mM -1 with a linear range from 0.3 to 1.5 mM; its fundamental analytical parameters were studied using a commercial soft drink. The obtained results proved sufficient repeatability (RSD = 1.9%), reproducibility (RSD = 2.5%), accuracy (95-105% recovery), and robustness (RSD = 3.3%). Furthermore, no significant interferences from fructose, ascorbic acid and citric acid were obtained. In addition, the storage stability was further examined, after 30 days, the GOx-Chitosan/TiO₂NTAs biosensor retained 85% of its initial current response. Finally, the glucose content of different food samples was measured using the biosensor and compared with the respective HPLC value. In the worst scenario, a deviation smaller than 10% was obtained among the 20 samples evaluated.

Water level management of lakes connected to regulated rivers: An integrated modeling and analytical methodology

Science.gov (United States)

Hu, Tengfei; Mao, Jingqiao; Pan, Shunqi; Dai, Lingquan; Zhang, Peipei; Xu, Diandian; Dai, Huichao

2018-07-01

Reservoir operations significantly alter the hydrological regime of the downstream river and river-connected lake, which has far-reaching impacts on the lake ecosystem. To facilitate the management of lakes connected to regulated rivers, the following information must be provided: (1) the response of lake water levels to reservoir operation schedules in the near future and (2) the importance of different rivers in terms of affecting the water levels in different lake regions of interest. We develop an integrated modeling and analytical methodology for the water level management of such lakes. The data-driven method is used to model the lake level as it has the potential of producing quick and accurate predictions. A new genetic algorithm-based synchronized search is proposed to optimize input variable time lags and data-driven model parameters simultaneously. The methodology also involves the orthogonal design and range analysis for extracting the influence of an individual river from that of all the rivers. The integrated methodology is applied to the second largest freshwater lake in China, the Dongting Lake. The results show that: (1) the antecedent lake levels are of crucial importance for the current lake level prediction; (2) the selected river discharge time lags reflect the spatial heterogeneity of the rivers' impacts on lake level changes; (3) the predicted lake levels are in very good agreement with the observed data (RMSE ≤ 0.091 m; R2 ≥ 0.9986). This study demonstrates the practical potential of the integrated methodology, which can provide both the lake level responses to future dam releases and the relative contributions of different rivers to lake level changes.

Study of New Analytical Methodologies for the Analysis of Polychlorinated Dibenzo-P-Dioxins (PCDDs) and Polychlorinated Di benzofurans (PCDFs) by Quadrupole Ion Storage Tandem-in-time Mass Spectrometry. Application to Environmental Samples; Estudio de nuevas metodologias analiticas en la determinacion de policlorodibenzo-P-dioxinas (PCDDs) y policlosrodibenzofuranos (PCDFs) por espectrometria de masas con trampa ionica. Aplicacion a muestras medioambientales

Energy Technology Data Exchange (ETDEWEB)

Sanz Chichon, M. P.

2008-07-01

Two alternative analytical methodologies have been developed for the analysis of polychlorinated dibenzo-p-dioxins (PCDDs) and di benzofurans (PCDFs) in environmental samples. The techniques studied have been: Pressurized Fluid Extraction (PFE) and Microwave-Assisted Extraction (MAE) versus Soxhlet extraction; the automated system Power-PrepTM versus the conventional cleanup using open chromatographic columns with different adsorbents and the application of tandem mass spectrometry (HRGC-MS/MS) versus high resolution mass spectrometry (HRGC-HRMS) for PCDD/Fs detection and quantification. (Author) 233 refs.

Diosgenin: Recent Highlights on Pharmacology and Analytical Methodology.

Science.gov (United States)

Jesus, Mafalda; Martins, Ana P J; Gallardo, Eugenia; Silvestre, Samuel

2016-01-01

Diosgenin, a steroidal sapogenin, occurs abundantly in plants such as Dioscorea alata , Smilax China, and Trigonella foenum graecum . This bioactive phytochemical not only is used as an important starting material for the preparation of several steroidal drugs in the pharmaceutical industry, but has revealed also high potential and interest in the treatment of various types of disorders such as cancer, hypercholesterolemia, inflammation, and several types of infections. Due to its pharmacological and industrial importance, several extraction and analytical procedures have been developed and applied over the years to isolate, detect, and quantify diosgenin, not only in its natural sources and pharmaceutical compositions, but also in animal matrices for pharmacodynamic, pharmacokinetic, and toxicological studies. Within these, HPLC technique coupled to different detectors is the most commonly analytical procedure described for this compound. However, other alternative methods were also published. Thus, the present review aims to provide collective information on the most recent pharmacological data on diosgenin and on the most relevant analytical techniques used to isolate, detect, and quantify this compound as well.

Diosgenin: Recent Highlights on Pharmacology and Analytical Methodology

Directory of Open Access Journals (Sweden)

Mafalda Jesus

2016-01-01

Full Text Available Diosgenin, a steroidal sapogenin, occurs abundantly in plants such as Dioscorea alata, Smilax China, and Trigonella foenum graecum. This bioactive phytochemical not only is used as an important starting material for the preparation of several steroidal drugs in the pharmaceutical industry, but has revealed also high potential and interest in the treatment of various types of disorders such as cancer, hypercholesterolemia, inflammation, and several types of infections. Due to its pharmacological and industrial importance, several extraction and analytical procedures have been developed and applied over the years to isolate, detect, and quantify diosgenin, not only in its natural sources and pharmaceutical compositions, but also in animal matrices for pharmacodynamic, pharmacokinetic, and toxicological studies. Within these, HPLC technique coupled to different detectors is the most commonly analytical procedure described for this compound. However, other alternative methods were also published. Thus, the present review aims to provide collective information on the most recent pharmacological data on diosgenin and on the most relevant analytical techniques used to isolate, detect, and quantify this compound as well.

Direct trace-elemental analysis of urine samples by laser ablation-inductively coupled plasma mass spectrometry after sample deposition on clinical filter papers.

Science.gov (United States)

Aramendía, Maite; Rello, Luis; Vanhaecke, Frank; Resano, Martín

2012-10-16

Collection of biological fluids on clinical filter papers shows important advantages from a logistic point of view, although analysis of these specimens is far from straightforward. Concerning urine analysis, and particularly when direct trace elemental analysis by laser ablation-inductively coupled plasma mass spectrometry (LA-ICPMS) is aimed at, several problems arise, such as lack of sensitivity or different distribution of the analytes on the filter paper, rendering obtaining reliable quantitative results quite difficult. In this paper, a novel approach for urine collection is proposed, which circumvents many of these problems. This methodology consists on the use of precut filter paper discs where large amounts of sample can be retained upon a single deposition. This provides higher amounts of the target analytes and, thus, sufficient sensitivity, and allows addition of an adequate internal standard at the clinical lab prior to analysis, therefore making it suitable for a strategy based on unsupervised sample collection and ulterior analysis at referral centers. On the basis of this sampling methodology, an analytical method was developed for the direct determination of several elements in urine (Be, Bi, Cd, Co, Cu, Ni, Sb, Sn, Tl, Pb, and V) at the low μg L(-1) level by means of LA-ICPMS. The method developed provides good results in terms of accuracy and LODs (≤1 μg L(-1) for most of the analytes tested), with a precision in the range of 15%, fit-for-purpose for clinical control analysis.

Pesticides residues in water treatment plant sludge: validation of analytical methodology using liquid chromatography coupled to Tandem mass spectrometry (LC-MS/MS)

International Nuclear Information System (INIS)

Moracci, Luiz Fernando Soares

2008-01-01

The evolving scenario of Brazilian agriculture brings benefits to the population and demands technological advances to this field. Constantly, new pesticides are introduced encouraging scientific studies with the aim of determine and evaluate impacts on the population and on environment. In this work, the evaluated sample was the sludge resulted from water treatment plant located in the Vale do Ribeira, Sao Paulo, Brazil. The technique used was the reversed phase liquid chromatography coupled to electrospray ionization tandem mass spectrometry. Compounds were previously liquid extracted from the matrix. The development of the methodology demanded data processing in order to be transformed into reliable information. The processes involved concepts of validation of chemical analysis. The evaluated parameters were selectivity, linearity, range, sensitivity, accuracy, precision, limit of detection, limit of quantification and robustness. The obtained qualitative and quantitative results were statistically treated and presented. The developed and validated methodology is simple. As results, even exploring the sensitivity of the analytical technique, the work compounds were not detected in the sludge of the WTP. One can explain that these compounds can be present in a very low concentration, can be degraded under the conditions of the water treatment process or are not completely retained by the WTP. (author)

Use of Cdse/ZnS quantum dots for sensitive detection and quantification of paraquat in water samples

Energy Technology Data Exchange (ETDEWEB)

Durán, Gema M. [Department of Analytical Chemistry and Food Technology, University of Castilla – La Mancha, Avenida Camilo José Cela, 10, 13004 Ciudad Real (Spain); IRICA (Regional Institute of Applied Scientific Research), Avenida Camilo José Cela, s/n., 13071 Ciudad Real (Spain); Contento, Ana M. [Department of Analytical Chemistry and Food Technology, University of Castilla – La Mancha, Avenida Camilo José Cela, 10, 13004 Ciudad Real (Spain); Ríos, Ángel, E-mail: Angel.Rios@uclm.es [Department of Analytical Chemistry and Food Technology, University of Castilla – La Mancha, Avenida Camilo José Cela, 10, 13004 Ciudad Real (Spain)

2013-11-01

Graphical abstract: -- Highlights: •Analytical use of CdSe/ZnS quantum dots. •Methodology for water solubilization of CdSe/ZnS QDs. •Sensitive and selective reaction with paraquat herbicide. •Application to water samples. -- Abstract: Based on the highly sensitive fluorescence change of water-soluble CdSe/ZnS core-shell quantum dots (QD) by paraquat herbicide, a simple, rapid and reproducible methodology was developed to selectively determine paraquat (PQ) in water samples. The methodology enabled the use of simple pretreatment procedure based on the simple water solubilization of CdSe/ZnS QDs with hydrophilic heterobifunctional thiol ligands, such as 3-mercaptopropionic acid (3-MPA), using microwave irradiation. The resulting water-soluble QDs exhibit a strong fluorescence emission at 596 nm with a high and reproducible photostability. The proposed analytical method thus satisfies the need for a simple, sensible and rapid methodology to determine residues of paraquat in water samples, as required by the increasingly strict regulations for health protection introduced in recent years. The sensitivity of the method, expressed as detection limits, was as low as 3.0 ng L{sup −1}. The lineal range was between 10–5 × 10{sup 3} ng L{sup −1}. RSD values in the range of 71–102% were obtained. The analytical applicability of proposed method was demonstrated by analyzing water samples from different procedence.

Use of Cdse/ZnS quantum dots for sensitive detection and quantification of paraquat in water samples

International Nuclear Information System (INIS)

Durán, Gema M.; Contento, Ana M.; Ríos, Ángel

2013-01-01

Graphical abstract: -- Highlights: •Analytical use of CdSe/ZnS quantum dots. •Methodology for water solubilization of CdSe/ZnS QDs. •Sensitive and selective reaction with paraquat herbicide. •Application to water samples. -- Abstract: Based on the highly sensitive fluorescence change of water-soluble CdSe/ZnS core-shell quantum dots (QD) by paraquat herbicide, a simple, rapid and reproducible methodology was developed to selectively determine paraquat (PQ) in water samples. The methodology enabled the use of simple pretreatment procedure based on the simple water solubilization of CdSe/ZnS QDs with hydrophilic heterobifunctional thiol ligands, such as 3-mercaptopropionic acid (3-MPA), using microwave irradiation. The resulting water-soluble QDs exhibit a strong fluorescence emission at 596 nm with a high and reproducible photostability. The proposed analytical method thus satisfies the need for a simple, sensible and rapid methodology to determine residues of paraquat in water samples, as required by the increasingly strict regulations for health protection introduced in recent years. The sensitivity of the method, expressed as detection limits, was as low as 3.0 ng L −1 . The lineal range was between 10–5 × 10 3 ng L −1 . RSD values in the range of 71–102% were obtained. The analytical applicability of proposed method was demonstrated by analyzing water samples from different procedence

Are marketed topical metronidazole creams bioequivalent? Evaluation by in vivo microdialysis sampling and tape stripping methodology

DEFF Research Database (Denmark)

Garcia Ortiz, Patricia Elodia; Hansen, S H; Shah, Surendra P.

2011-01-01

To evaluate the bioequivalence of 3 marketed topical metronidazole formulations by simultaneous dermal microdialysis and stratum corneum sampling by the tape stripping methodology, and to compare the techniques as tools for the determination of bioequivalence.......To evaluate the bioequivalence of 3 marketed topical metronidazole formulations by simultaneous dermal microdialysis and stratum corneum sampling by the tape stripping methodology, and to compare the techniques as tools for the determination of bioequivalence....

Study of adolescents exposed in utero. Methodological evaluation of the Nagasaki sample

Energy Technology Data Exchange (ETDEWEB)

Hrubec, Zdenek, Noble, K.B.; Burrow, G N

1962-09-12

Fetal tissues have been shown to be extremely sensitive to ionizing radiation, and therefore a group of children who were exposed in utero are of special interest. When these children entered adolescence, an intensive study was undertaken to determine whether differences not otherwise apparent would be revealed during the stress of this period of rapid growth. The purpose of this report is to describe the sample used to study these adolescent children who were exposed in utero and to provide reference information. The problems of using ex post facto methods as employed in this study have been discussed in detail elsewhere. In summary, the extent to which findings of a retrospective study may be generalized to a larger population can be determined only from a careful and extensive study of the characteristics of the sample and an evaluation of the procedures used in its selection. It is generally recognized that even an extensive methodologic exploration of this kind offers no conclusive proof that a sample is useful for a specific study. In the sample, some variables which may have a considerable effect on the medical data, such as socioeconomic status, have been taken into account only superficially. There is always the possibility that some important, completely unsuspected variables may produce spurious associations. However there is an almost infinite number of such factors which might conceivably affect the data. Vast research resources could be committed to a methodologic evaluation without fulfilling the basic purpose of the study. An approach must be devised which is judged methodologically adequate but which will not tax the research resource to the detriment of the basic objectives. It is hoped that this report will satisfy the requirements of this compromise. 30 references, 36 tables.

Analytical procedures for determining Pb and Sr isotopic compositions in water samples by ID-TIMS

Directory of Open Access Journals (Sweden)

Veridiana Martins

2008-01-01

Full Text Available Few articles deal with lead and strontium isotopic analysis of water samples. The aim of this study was to define the chemical procedures for Pb and Sr isotopic analyses of groundwater samples from an urban sedimentary aquifer. Thirty lead and fourteen strontium isotopic analyses were performed to test different analytical procedures. Pb and Sr isotopic ratios as well as Sr concentration did not vary using different chemical procedures. However, the Pb concentrations were very dependent on the different procedures. Therefore, the choice of the best analytical procedure was based on the Pb results, which indicated a higher reproducibility from samples that had been filtered and acidified before the evaporation, had their residues totally dissolved, and were purified by ion chromatography using the Biorad® column. Our results showed no changes in Pb ratios with the storage time.

Analytical methodologies based on LC-MS/MS for monitoring selected emerging compounds in liquid and solid phases of the sewage sludge.

Science.gov (United States)

Boix, C; Ibáñez, M; Fabregat-Safont, D; Morales, E; Pastor, L; Sancho, J V; Sánchez-Ramírez, J E; Hernández, F

2016-01-01

In this work, two analytical methodologies based on liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) were developed for quantification of emerging pollutants identified in sewage sludge after a previous wide-scope screening. The target list included 13 emerging contaminants (EC): thiabendazole, acesulfame, fenofibric acid, valsartan, irbesartan, salicylic acid, diclofenac, carbamazepine, 4-aminoantipyrine (4-AA), 4-acetyl aminoantipyrine (4-AAA), 4-formyl aminoantipyrine (4-FAA), venlafaxine and benzoylecgonine. The aqueous and solid phases of the sewage sludge were analyzed making use of Solid-Phase Extraction (SPE) and UltraSonic Extraction (USE) for sample treatment, respectively. The methods were validated at three concentration levels: 0.2, 2 and 20 μg L(-1) for the aqueous phase, and 50, 500 and 2000 μg kg(-1) for the solid phase of the sludge. In general, the method was satisfactorily validated, showing good recoveries (70-120%) and precision (RSD metabolites of dipyrone had not been studied before in sewage sludge.

Validação de metodologia analítica para doseamento de soluções de lapachol por CLAE Validation of the analytical methodology for evaluation of lapachol in solution by HPCL

Directory of Open Access Journals (Sweden)

Said G. C. Fonseca

2004-02-01

Full Text Available Lapachol is a naphthoquinone found in several species of the Bignoniaceae family possessing mainly anticancer activity. The present work consists of the development and validation of analytical methodology for lapachol and its preparations. The results here obtained show that lapachol has a low quantification limit, that the analytical methodology is accurate, reproducible, robust and linear over the concentration range 0.5-100 µg/mL of lapachol.

A review of electro analytical determinations of some important elements (Zn, Se, As) in environmental samples

International Nuclear Information System (INIS)

Lichiang; James, B.D.; Magee, R.J.

1991-01-01

This review covers electro analytical methods reported in the literature for the determination of zinc, cadmium, selenium and arsenic in environmental and biological samples. A comprehensive survey of electro analytical techniques used for the determination of four important elements, i.e. zinc, cadmium, selenium and arsenic is reported herein with 322 references up to 1990. (Orig./A.B.)

Dietary exposure to trace elements and radionuclides: the methodology of the Italian total diet study 2012-2014

Directory of Open Access Journals (Sweden)

Marilena D'Amato

2013-09-01

Full Text Available This article presents the methodology of the Italian Total Diet Study 2012-2014 aimed at assessing the dietary exposure of the general Italian population to selected non-essential trace elements (Al, inorganic As, Cd, Pb, methyl-Hg, inorganic Hg, U and radionuclides (40K, 134Cs, 137Cs, 90Sr. The establishment of the TDS food list, the design of the sampling plan, and details about the collection of food samples, their standardized culinary treatment, pooling into analytical samples and subsequent sample treatment are described. Analytical techniques and quality assurance are discussed, with emphasis on the need for speciation data and for minimizing the percentage of left-censored data so as to reduce uncertainties in exposure assessment. Finally the methodology for estimating the exposure of the general population and of population subgroups according to age (children, teenagers, adults, and the elderly and gender, both at the national level and for each of the four main geographical areas of Italy, is presented.

Analytical results from salt batch 9 routine DSSHT and SEHT monthly samples

Energy Technology Data Exchange (ETDEWEB)

Peters, T. B. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

2017-06-01

Strip Effluent Hold Tank (SEHT) and Decontaminated Salt Solution Hold Tank (DSSHT) samples from several of the “microbatches” of Integrated Salt Disposition Project (ISDP) Salt Batch (“Macrobatch”) 9 have been analyzed for ²³⁸Pu, ⁹⁰Sr, ¹³⁷Cs, cations (Inductively Coupled Plasma Emission Spectroscopy - ICPES), and anions (Ion Chromatography Anions - IC-A). The analytical results from the current microbatch samples are similar to those from previous macrobatch samples. The Cs removal continues to be acceptable, with decontamination factors (DF) averaging 25700 (107% RSD). The bulk chemistry of the DSSHT and SEHT samples do not show any signs of unusual behavior, other than lacking the anticipated degree of dilution that is calculated to occur during Modular Caustic-Side Solvent Extraction Unit (MCU) processing.

ANALYTICAL ANARCHISM: THE PROBLEM OF DEFINITION AND DEMARCATION

OpenAIRE

Konstantinov M.S.

2012-01-01

In this paper the first time in the science of our country is considered a new trend of anarchist thought - analytical anarchism. As a methodological tool used critical analysis of the key propositions of the basic versions of this trend: the anarcho- capitalist and egalitarian. The study was proposed classification of discernible trends within the analytical anarchism on the basis of value criteria, identified conceptual and methodological problems of definition analytical anarchism and its ...

New materials for sample preparation techniques in bioanalysis.

Science.gov (United States)

Nazario, Carlos Eduardo Domingues; Fumes, Bruno Henrique; da Silva, Meire Ribeiro; Lanças, Fernando Mauro

2017-02-01

The analysis of biological samples is a complex and difficult task owing to two basic and complementary issues: the high complexity of most biological matrices and the need to determine minute quantities of active substances and contaminants in such complex sample. To succeed in this endeavor samples are usually subject to three steps of a comprehensive analytical methodological approach: sample preparation, analytes isolation (usually utilizing a chromatographic technique) and qualitative/quantitative analysis (usually with the aid of mass spectrometric tools). Owing to the complex nature of bio-samples, and the very low concentration of the target analytes to be determined, selective sample preparation techniques is mandatory in order to overcome the difficulties imposed by these two constraints. During the last decade new chemical synthesis approaches has been developed and optimized, such as sol-gel and molecularly imprinting technologies, allowing the preparation of novel materials for sample preparation including graphene and derivatives, magnetic materials, ionic liquids, molecularly imprinted polymers, and much more. In this contribution we will review these novel techniques and materials, as well as their application to the bioanalysis niche. Copyright © 2016 Elsevier B.V. All rights reserved.

Recent bibliography on analytical and sampling problems of a PWR primary coolant Suppl. 4

International Nuclear Information System (INIS)

Illy, H.

1986-09-01

The 4th supplement of a bibliographical series comprising the analytical and sampling problems of the primary coolant of PWR type reactors covers the literature from 1985 up to July 1986 (220 items). References are listed according to the following topics: boric acid; chloride, chlorine; general; hydrogen isotopes; iodine; iodide; noble gases; oxygen; other elements; radiation monitoring; reactor safety; sampling; water chemistry. (V.N.)

Analytical Parameters of an Amperometric Glucose Biosensor for Fast Analysis in Food Samples

Directory of Open Access Journals (Sweden)

Margalida Artigues

2017-11-01

Full Text Available Amperometric biosensors based on the use of glucose oxidase (GOx are able to combine the robustness of electrochemical techniques with the specificity of biological recognition processes. However, very little information can be found in literature about the fundamental analytical parameters of these sensors. In this work, the analytical behavior of an amperometric biosensor based on the immobilization of GOx using a hydrogel (Chitosan onto highly ordered titanium dioxide nanotube arrays (TiO2NTAs has been evaluated. The GOx–Chitosan/TiO2NTAs biosensor showed a sensitivity of 5.46 μA·mM−1 with a linear range from 0.3 to 1.5 mM; its fundamental analytical parameters were studied using a commercial soft drink. The obtained results proved sufficient repeatability (RSD = 1.9%, reproducibility (RSD = 2.5%, accuracy (95–105% recovery, and robustness (RSD = 3.3%. Furthermore, no significant interferences from fructose, ascorbic acid and citric acid were obtained. In addition, the storage stability was further examined, after 30 days, the GOx–Chitosan/TiO2NTAs biosensor retained 85% of its initial current response. Finally, the glucose content of different food samples was measured using the biosensor and compared with the respective HPLC value. In the worst scenario, a deviation smaller than 10% was obtained among the 20 samples evaluated.

Analytical Parameters of an Amperometric Glucose Biosensor for Fast Analysis in Food Samples

Science.gov (United States)

2017-01-01

Amperometric biosensors based on the use of glucose oxidase (GOx) are able to combine the robustness of electrochemical techniques with the specificity of biological recognition processes. However, very little information can be found in literature about the fundamental analytical parameters of these sensors. In this work, the analytical behavior of an amperometric biosensor based on the immobilization of GOx using a hydrogel (Chitosan) onto highly ordered titanium dioxide nanotube arrays (TiO2NTAs) has been evaluated. The GOx–Chitosan/TiO2NTAs biosensor showed a sensitivity of 5.46 μA·mM−1 with a linear range from 0.3 to 1.5 mM; its fundamental analytical parameters were studied using a commercial soft drink. The obtained results proved sufficient repeatability (RSD = 1.9%), reproducibility (RSD = 2.5%), accuracy (95–105% recovery), and robustness (RSD = 3.3%). Furthermore, no significant interferences from fructose, ascorbic acid and citric acid were obtained. In addition, the storage stability was further examined, after 30 days, the GOx–Chitosan/TiO2NTAs biosensor retained 85% of its initial current response. Finally, the glucose content of different food samples was measured using the biosensor and compared with the respective HPLC value. In the worst scenario, a deviation smaller than 10% was obtained among the 20 samples evaluated. PMID:29135931

Intercalibration of analytical methods on marine environmental samples

International Nuclear Information System (INIS)

1988-06-01

The pollution of the seas by various chemical substances constitutes nowadays one of the principal concerns of mankind. The International Atomic Energy Agency has organized in past years several intercomparison exercises in the framework of its Analytical Quality Control Service. The present intercomparison had a double aim: first, to give laboratories participating in this intercomparison an opportunity for checking their analytical performance. Secondly, to produce on the basis of the results of this intercomparison a reference material made of fish tissue which would be accurately certified with respect to many trace elements. Such a material could be used by analytical chemists to check the validity of new analytical procedures. In total, 53 laboratories from 29 countries reported results (585 laboratory means for 48 elements). 5 refs, 52 tabs

Validated analytical methodology for the simultaneous determination of a wide range of pesticides in human blood using GC-MS/MS and LC-ESI/MS/MS and its application in two poisoning cases.

Science.gov (United States)

Luzardo, Octavio P; Almeida-González, Maira; Ruiz-Suárez, Norberto; Zumbado, Manuel; Henríquez-Hernández, Luis A; Meilán, María José; Camacho, María; Boada, Luis D

2015-09-01

Pesticides are frequently responsible for human poisoning and often the information on the involved substance is lacking. The great variety of pesticides that could be responsible for intoxication makes necessary the development of powerful and versatile analytical methodologies, which allows the identification of the unknown toxic substance. Here we developed a methodology for simultaneous identification and quantification in human blood of 109 highly toxic pesticides. The application of this analytical scheme would help in minimizing the cost of this type of chemical identification, maximizing the chances of identifying the pesticide involved. In the methodology that we present here, we use a liquid-liquid extraction, followed by one single purification step, and quantitation of analytes by a combination of liquid and gas chromatography, both coupled to triple quadrupole mass spectrometry, which is operated in the mode of multiple reaction monitoring. The methodology has been fully validated, and its applicability has been demonstrated in two recent cases involving one self-poisoning fatality and one non-fatal homicidal attempt. Copyright © 2015 The Chartered Society of Forensic Sciences. Published by Elsevier Ireland Ltd. All rights reserved.

A solid phase extraction-ion chromatography with conductivity detection procedure for determining cationic surfactants in surface water samples.

Science.gov (United States)

Olkowska, Ewa; Polkowska, Żaneta; Namieśnik, Jacek

2013-11-15

A new analytical procedure for the simultaneous determination of individual cationic surfactants (alkyl benzyl dimethyl ammonium chlorides) in surface water samples has been developed. We describe this methodology for the first time: it involves the application of solid phase extraction (SPE-for sample preparation) coupled with ion chromatography-conductivity detection (IC-CD-for the final determination). Mean recoveries of analytes between 79% and 93%, and overall method quantification limits in the range from 0.0018 to 0.038 μg/mL for surface water and CRM samples were achieved. The methodology was applied to the determination of individual alkyl benzyl quaternary ammonium compounds in environmental samples (reservoir water) and enables their presence in such types of waters to be confirmed. In addition, it is a simpler, less time-consuming, labour-intensive, avoiding use of toxic chloroform and significantly less expensive methodology than previously described approaches (liquid-liquid extraction coupled with liquid chromatography-mass spectrometry). Copyright © 2013 Elsevier B.V. All rights reserved.

Voltammetric technique, a panacea for analytical examination of environmental samples

International Nuclear Information System (INIS)

Zahir, E.; Mohiuddin, S.; Naqvi, I.I.

2012-01-01

Voltammetric methods for trace metal analysis in environmental samples of marine origin like mangrove, sediments and shrimps are generally recommended. Three different electro-analytical techniques i.e. polarography, anodic stripping voltammetry (ASV) and adsorptive stripping voltammetry (ADSV) have been used. Cd/sub 2/+, Pb/sub 2/+, Cu/sub 2/+ and Mn/sub 2/+ were determined through ASV, Cr/sub 6/+ was analyzed by ADSV and Fe/sub 2/+, Zn/sub 2/+, Ni/sub 2/+ and Co/sub 2/+ were determined through polarography. Out of which pairs of Fe/sub 2/+Zn/sub 2/+ and Ni/sub 2/+Co/sub 2/+ were determined in two separate runs while Cd/sub 2/+, Pb/sub 2/+, Cu/sub 2/+ were analyzed in single run of ASV. Sensitivity and speciation capabilities of voltammetric methods have been employed. Analysis conditions were optimized that includes selection of supporting electrolyte, pH, working electrodes, sweep rate etc. Stripping voltammetry was adopted for analysis at ultra trace levels. Statistical parameters for analytical method development like selectivity factor, interference, repeatability (0.0065-0.130 macro g/g), reproducibility (0.08125-1.625 macro g/g), detection limits (0.032-5.06 macro g/g), limits of quantification (0.081-12.652 macro g/g), sensitivities (5.636-2.15 nA mL macro g-1) etc. were also determined. The percentage recoveries were found in between 95-105% using certified reference materials. Real samples of complex marine environment from Karachi coastline were also analyzed. The standard addition method was employed where any matrix effect was evidenced. (author)

Reference Intervals of Common Clinical Chemistry Analytes for Adults in Hong Kong.

Science.gov (United States)

Lo, Y C; Armbruster, David A

2012-04-01

Defining reference intervals is a major challenge because of the difficulty in recruiting volunteers to participate and testing samples from a significant number of healthy reference individuals. Historical literature citation intervals are often suboptimal because they're be based on obsolete methods and/or only a small number of poorly defined reference samples. Blood donors in Hong Kong gave permission for additional blood to be collected for reference interval testing. The samples were tested for twenty-five routine analytes on the Abbott ARCHITECT clinical chemistry system. Results were analyzed using the Rhoads EP evaluator software program, which is based on the CLSI/IFCC C28-A guideline, and defines the reference interval as the 95% central range. Method specific reference intervals were established for twenty-five common clinical chemistry analytes for a Chinese ethnic population. The intervals were defined for each gender separately and for genders combined. Gender specific or combined gender intervals were adapted as appropriate for each analyte. A large number of healthy, apparently normal blood donors from a local ethnic population were tested to provide current reference intervals for a new clinical chemistry system. Intervals were determined following an accepted international guideline. Laboratories using the same or similar methodologies may adapt these intervals if deemed validated and deemed suitable for their patient population. Laboratories using different methodologies may be able to successfully adapt the intervals for their facilities using the reference interval transference technique based on a method comparison study.

Collaborative Visual Analytics: A Health Analytics Approach to Injury Prevention

Directory of Open Access Journals (Sweden)

Samar Al-Hajj

2017-09-01

Full Text Available Background: Accurate understanding of complex health data is critical in order to deal with wicked health problems and make timely decisions. Wicked problems refer to ill-structured and dynamic problems that combine multidimensional elements, which often preclude the conventional problem solving approach. This pilot study introduces visual analytics (VA methods to multi-stakeholder decision-making sessions about child injury prevention; Methods: Inspired by the Delphi method, we introduced a novel methodology—group analytics (GA. GA was pilot-tested to evaluate the impact of collaborative visual analytics on facilitating problem solving and supporting decision-making. We conducted two GA sessions. Collected data included stakeholders’ observations, audio and video recordings, questionnaires, and follow up interviews. The GA sessions were analyzed using the Joint Activity Theory protocol analysis methods; Results: The GA methodology triggered the emergence of ‘common ground’ among stakeholders. This common ground evolved throughout the sessions to enhance stakeholders’ verbal and non-verbal communication, as well as coordination of joint activities and ultimately collaboration on problem solving and decision-making; Conclusions: Understanding complex health data is necessary for informed decisions. Equally important, in this case, is the use of the group analytics methodology to achieve ‘common ground’ among diverse stakeholders about health data and their implications.

A review of analytical techniques for the determination of carbon-14 in environmental samples

International Nuclear Information System (INIS)

Milton, G.M.; Brown, R.M.

1993-11-01

This report contains a brief summary of analytical techniques commonly used for the determination of radiocarbon in a variety of environmental samples. Details of the applicable procedures developed and tested in the Environmental Research Branch at Chalk River Laboratories are appended

Analysis of plant gums and saccharide materials in paint samples: comparison of GC-MS analytical procedures and databases.

Science.gov (United States)

Lluveras-Tenorio, Anna; Mazurek, Joy; Restivo, Annalaura; Colombini, Maria Perla; Bonaduce, Ilaria

2012-10-10

Saccharide materials have been used for centuries as binding media, to paint, write and illuminate manuscripts and to apply metallic leaf decorations. Although the technical literature often reports on the use of plant gums as binders, actually several other saccharide materials can be encountered in paint samples, not only as major binders, but also as additives. In the literature, there are a variety of analytical procedures that utilize GC-MS to characterize saccharide materials in paint samples, however the chromatographic profiles are often extremely different and it is impossible to compare them and reliably identify the paint binder. This paper presents a comparison between two different analytical procedures based on GC-MS for the analysis of saccharide materials in works-of-art. The research presented here evaluates the influence of the analytical procedure used, and how it impacts the sugar profiles obtained from the analysis of paint samples that contain saccharide materials. The procedures have been developed, optimised and systematically used to characterise plant gums at the Getty Conservation Institute in Los Angeles, USA (GCI) and the Department of Chemistry and Industrial Chemistry of the University of Pisa, Italy (DCCI). The main steps of the analytical procedures and their optimisation are discussed. The results presented highlight that the two methods give comparable sugar profiles, whether the samples analysed are simple raw materials, pigmented and unpigmented paint replicas, or paint samples collected from hundreds of centuries old polychrome art objects. A common database of sugar profiles of reference materials commonly found in paint samples was thus compiled. The database presents data also from those materials that only contain a minor saccharide fraction. This database highlights how many sources of saccharides can be found in a paint sample, representing an important step forward in the problem of identifying polysaccharide binders in

Headspace mass spectrometry methodology: application to oil spill identification in soils

Energy Technology Data Exchange (ETDEWEB)

Perez Pavon, J.L.; Garcia Pinto, C.; Moreno Cordero, B. [Universidad de Salamanca, Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias Quimicas, Salamanca (Spain); Guerrero Pena, A. [Universidad de Salamanca, Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias Quimicas, Salamanca (Spain); Laboratorio de Suelos, Plantas y Aguas, Campus Tabasco, Colegio de Postgraduados, Cardenas, Tabasco (Mexico)

2008-05-15

In the present work we report the results obtained with a methodology based on direct coupling of a headspace generator to a mass spectrometer for the identification of different types of petroleum crudes in polluted soils. With no prior treatment, the samples are subjected to the headspace generation process and the volatiles generated are introduced directly into the mass spectrometer, thereby obtaining a fingerprint of volatiles in the sample analysed. The mass spectrum corresponding to the mass/charge ratios (m/z) contains the information related to the composition of the headspace and is used as the analytical signal for the characterization of the samples. The signals obtained for the different samples were treated by chemometric techniques to obtain the desired information. The main advantage of the proposed methodology is that no prior chromatographic separation and no sample manipulation are required. The method is rapid, simple and, in view of the results, highly promising for the implementation of a new approach for oil spill identification in soils. (orig.)

Analytical methodologies based on LC–MS/MS for monitoring selected emerging compounds in liquid and solid phases of the sewage sludge

OpenAIRE

Boix Sales, Clara; Ibáñez Martínez, María; Fabregat-Safont, David; Morales, E.; Pastor, L.; Sancho Llopis, Juan Vicente; Sánchez-Ramírez, J. E.; Hernández Hernández, Félix

2016-01-01

In this work, two analytical methodologies based on liquid chromatography coupled to tandem mass spectrometry (LC–MS/MS) were developed for quantification of emerging pollutants identified in sewage sludge after a previous wide-scope screening. The target list included 13 emerging contaminants (EC): thiabendazole, acesulfame, fenofibric acid, valsartan, irbesartan, salicylic acid, diclofenac, carbamazepine, 4-aminoantipyrine (4- AA), 4-acetyl aminoantipyrine (4-AAA), 4-formyl amin...

Analytical methodologies based on LC?MS/MS for monitoring selected emerging compounds in liquid and solid phases of the sewage sludge

OpenAIRE

Boix, C.; Ib??ez, M.; Fabregat-Safont, D.; Morales, E.; Pastor, L.; Sancho, J.V.; S?nchez-Ram?rez, J.E.; Hern?ndez, F.

2016-01-01

In this work, two analytical methodologies based on liquid chromatography coupled to tandem mass spectrometry (LC?MS/MS) were developed for quantification of emerging pollutants identified in sewage sludge after a previous wide-scope screening. The target list included 13 emerging contaminants (EC): thiabendazole, acesulfame, fenofibric acid, valsartan, irbesartan, salicylic acid, diclofenac, carbamazepine, 4-aminoantipyrine (4-AA), 4-acetyl aminoantipyrine (4-AAA), 4-formyl aminoantipyrine (...

Analytical group decision making in natural resources: Methodology and application

Science.gov (United States)

Schmoldt, D.L.; Peterson, D.L.

2000-01-01

Group decision making is becoming increasingly important in natural resource management and associated scientific applications, because multiple values are treated coincidentally in time and space, multiple resource specialists are needed, and multiple stakeholders must be included in the decision process. Decades of social science research on decision making in groups have provided insights into the impediments to effective group processes and on techniques that can be applied in a group context. Nevertheless, little integration and few applications of these results have occurred in resource management decision processes, where formal groups are integral, either directly or indirectly. A group decision-making methodology is introduced as an effective approach for temporary, formal groups (e.g., workshops). It combines the following three components: (1) brainstorming to generate ideas; (2) the analytic hierarchy process to produce judgments, manage conflict, enable consensus, and plan for implementation; and (3) a discussion template (straw document). Resulting numerical assessments of alternative decision priorities can be analyzed statistically to indicate where group member agreement occurs and where priority values are significantly different. An application of this group process to fire research program development in a workshop setting indicates that the process helps focus group deliberations; mitigates groupthink, nondecision, and social loafing pitfalls; encourages individual interaction; identifies irrational judgments; and provides a large amount of useful quantitative information about group preferences. This approach can help facilitate scientific assessments and other decision-making processes in resource management.

New high temperature plasmas and sample introduction systems for analytical atomic emission and mass spectrometry

International Nuclear Information System (INIS)

Montaser, A.

1993-01-01

In this research, new high-temperature plasmas and new sample introduction systems are explored for rapid elemental and isotopic analysis of gases, solutions, and solids using mass spectrometry and atomic emission spectrometry. During the period January 1993--December 1993, emphasis was placed on (a) analytical investigations of atmospheric-pressure helium inductively coupled plasma (He ICP) that are suitable for atomization, excitation, and ionization of elements possessing high excitation and ionization energies; (b) simulation and computer modeling of plasma sources to predict their structure and fundamental and analytical properties without incurring the enormous cost of experimental studies; (c) spectrosopic imaging and diagnostic studies of high-temperature plasmas; (d) fundamental studies of He ICP discharges and argon-nitrogen plasma by high-resolution Fourier transform spectrometry; and (e) fundamental and analytical investigation of new, low-cost devices as sample introduction systems for atomic spectrometry and examination of new diagnostic techniques for probing aerosols. Only the most important achievements are included in this report to illustrate progress and obstacles. Detailed descriptions of the authors' investigations are outlined in the reprints and preprints that accompany this report. The technical progress expected next year is briefly described at the end of this report

Tank 241-U-104 headspace gas and vapor characterization results from samples collected on July 16, 1996

International Nuclear Information System (INIS)

Pool, K.H.; Evans, J.C.; Hayes, J.C.; Mitroshkov, A.V.; Edwards, J.A.; Julya, J.L.; Thornton, B.M.; Fruchter, J.S.; Silvers, K.L.

1997-08-01

This report presents the results from analyses of samples taken from the headspace of waste storage tank 241-U-104 (Tank U-104) at the Hanford Site in Washington State. Tank headspace samples collected by Westinghouse Hanford Company (WHC) were analyzed by Pacific Northwest National Laboratory (PNNL) to determine headspace concentrations of selected non-radioactive analytes. Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Vapor concentrations from sorbent trap samples are based on measured sample volumes provided by WHC. No analytes were determined to be above the immediate notification limits specified by the sampling and analysis plan. None of the flammable constituents were present at concentrations above the analytical instrument detection limits. Total headspace flammability was estimated to be <0.108% of the lower flammability limit. Average measured concentrations of targeted gases, inorganic vapors, and selected organic vapors are provided in a table. A summary of experimental methods, including sampling methodology, analytical procedures, and quality assurance and control methods are presented in Section 2.0. Detailed descriptions of the analytical results are provided in Section 3.0

Development of numerical and analytical methodology for stress analysis in guide tubes of fuel elements

International Nuclear Information System (INIS)

Carrilho, Leo A.; Dotto, Rosvita M.; Gouvea, Jayme P. de

2000-01-01

The stresses in the components of fuel elements in operation have been calculated by Industrias Nucleares do Brasil - INB, using programmes specifically developed for this are. However, worldwide useful software as Excel and ANSYS have resources that make them an alternative with advantages for those computing. In this context, the stress and displacements were calculated in the guide thimbles of a fuel element in normal operation in the reactor under static loads, through analytic and numeric models, which results are comparable to that obtained with the actual INB's methodology. The discussion of the results exposes the peculiarity of a pick of compression stress in a segment of the guide thimble which is accentuated during low power operations. Suggestions for the relief of these high stresses are proposed for future studies. (author)

Net analyte signal based statistical quality control

NARCIS (Netherlands)

Skibsted, E.T.S.; Boelens, H.F.M.; Westerhuis, J.A.; Smilde, A.K.; Broad, N.W.; Rees, D.R.; Witte, D.T.

2005-01-01

Net analyte signal statistical quality control (NAS-SQC) is a new methodology to perform multivariate product quality monitoring based on the net analyte signal approach. The main advantage of NAS-SQC is that the systematic variation in the product due to the analyte (or property) of interest is

Comparing Classic and Interval Analytical Hierarchy Process Methodologies for Measuring Area-Level Deprivation to Analyze Health Inequalities.

Science.gov (United States)

Cabrera-Barona, Pablo; Ghorbanzadeh, Omid

2018-01-16

Deprivation indices are useful measures to study health inequalities. Different techniques are commonly applied to construct deprivation indices, including multi-criteria decision methods such as the analytical hierarchy process (AHP). The multi-criteria deprivation index for the city of Quito is an index in which indicators are weighted by applying the AHP. In this research, a variation of this index is introduced that is calculated using interval AHP methodology. Both indices are compared by applying logistic generalized linear models and multilevel models, considering self-reported health as the dependent variable and deprivation and self-reported quality of life as the independent variables. The obtained results show that the multi-criteria deprivation index for the city of Quito is a meaningful measure to assess neighborhood effects on self-reported health and that the alternative deprivation index using the interval AHP methodology more thoroughly represents the local knowledge of experts and stakeholders. These differences could support decision makers in improving health planning and in tackling health inequalities in more deprived areas.

Optimization of a Pre-MEKC Separation SPE Procedure for Steroid Molecules in Human Urine Samples

Directory of Open Access Journals (Sweden)

Ilona Olędzka

2013-11-01

Full Text Available Many steroid hormones can be considered as potential biomarkers and their determination in body fluids can create opportunities for the rapid diagnosis of many diseases and disorders of the human body. Most existing methods for the determination of steroids are usually time- and labor-consuming and quite costly. Therefore, the aim of analytical laboratories is to develop a new, relatively low-cost and rapid implementation methodology for their determination in biological samples. Due to the fact that there is little literature data on concentrations of steroid hormones in urine samples, we have made attempts at the electrophoretic determination of these compounds. For this purpose, an extraction procedure for the optimized separation and simultaneous determination of seven steroid hormones in urine samples has been investigated. The isolation of analytes from biological samples was performed by liquid-liquid extraction (LLE with dichloromethane and compared to solid phase extraction (SPE with C18 and hydrophilic-lipophilic balance (HLB columns. To separate all the analytes a micellar electrokinetic capillary chromatography (MECK technique was employed. For full separation of all the analytes a running buffer (pH 9.2, composed of 10 mM sodium tetraborate decahydrate (borax, 50 mM sodium dodecyl sulfate (SDS, and 10% methanol was selected. The methodology developed in this work for the determination of steroid hormones meets all the requirements of analytical methods. The applicability of the method has been confirmed for the analysis of urine samples collected from volunteers—both men and women (students, amateur bodybuilders, using and not applying steroid doping. The data obtained during this work can be successfully used for further research on the determination of steroid hormones in urine samples.

Analytical methods in sphingolipidomics: Quantitative and profiling approaches in food analysis.

Science.gov (United States)

Canela, Núria; Herrero, Pol; Mariné, Sílvia; Nadal, Pedro; Ras, Maria Rosa; Rodríguez, Miguel Ángel; Arola, Lluís

2016-01-08

In recent years, sphingolipidomics has emerged as an interesting omic science that encompasses the study of the full sphingolipidome characterization, content, structure and activity in cells, tissues or organisms. Like other omics, it has the potential to impact biomarker discovery, drug development and systems biology knowledge. Concretely, dietary food sphingolipids have gained considerable importance due to their extensively reported bioactivity. Because of the complexity of this lipid family and their diversity among foods, powerful analytical methodologies are needed for their study. The analytical tools developed in the past have been improved with the enormous advances made in recent years in mass spectrometry (MS) and chromatography, which allow the convenient and sensitive identification and quantitation of sphingolipid classes and form the basis of current sphingolipidomics methodologies. In addition, novel hyphenated nuclear magnetic resonance (NMR) strategies, new ionization strategies, and MS imaging are outlined as promising technologies to shape the future of sphingolipid analyses. This review traces the analytical methods of sphingolipidomics in food analysis concerning sample extraction, chromatographic separation, the identification and quantification of sphingolipids by MS and their structural elucidation by NMR. Copyright © 2015 Elsevier B.V. All rights reserved.

Analysis of environmental contamination resulting from catastrophic incidents: part 2. Building laboratory capability by selecting and developing analytical methodologies.

Science.gov (United States)

Magnuson, Matthew; Campisano, Romy; Griggs, John; Fitz-James, Schatzi; Hall, Kathy; Mapp, Latisha; Mullins, Marissa; Nichols, Tonya; Shah, Sanjiv; Silvestri, Erin; Smith, Terry; Willison, Stuart; Ernst, Hiba

2014-11-01

Catastrophic incidents can generate a large number of samples of analytically diverse types, including forensic, clinical, environmental, food, and others. Environmental samples include water, wastewater, soil, air, urban building and infrastructure materials, and surface residue. Such samples may arise not only from contamination from the incident but also from the multitude of activities surrounding the response to the incident, including decontamination. This document summarizes a range of activities to help build laboratory capability in preparation for sample analysis following a catastrophic incident, including selection and development of fit-for-purpose analytical methods for chemical, biological, and radiological contaminants. Fit-for-purpose methods are those which have been selected to meet project specific data quality objectives. For example, methods could be fit for screening contamination in the early phases of investigation of contamination incidents because they are rapid and easily implemented, but those same methods may not be fit for the purpose of remediating the environment to acceptable levels when a more sensitive method is required. While the exact data quality objectives defining fitness-for-purpose can vary with each incident, a governing principle of the method selection and development process for environmental remediation and recovery is based on achieving high throughput while maintaining high quality analytical results. This paper illustrates the result of applying this principle, in the form of a compendium of analytical methods for contaminants of interest. The compendium is based on experience with actual incidents, where appropriate and available. This paper also discusses efforts aimed at adaptation of existing methods to increase fitness-for-purpose and development of innovative methods when necessary. The contaminants of interest are primarily those potentially released through catastrophes resulting from malicious activity

Macro elemental analysis of food samples by nuclear analytical technique

Science.gov (United States)

Syahfitri, W. Y. N.; Kurniawati, S.; Adventini, N.; Damastuti, E.; Lestiani, D. D.

2017-06-01

Energy-dispersive X-ray fluorescence (EDXRF) spectrometry is a non-destructive, rapid, multi elemental, accurate, and environment friendly analysis compared with other detection methods. Thus, EDXRF spectrometry is applicable for food inspection. The macro elements calcium and potassium constitute important nutrients required by the human body for optimal physiological functions. Therefore, the determination of Ca and K content in various foods needs to be done. The aim of this work is to demonstrate the applicability of EDXRF for food analysis. The analytical performance of non-destructive EDXRF was compared with other analytical techniques; neutron activation analysis and atomic absorption spectrometry. Comparison of methods performed as cross checking results of the analysis and to overcome the limitations of the three methods. Analysis results showed that Ca found in food using EDXRF and AAS were not significantly different with p-value 0.9687, whereas p-value of K between EDXRF and NAA is 0.6575. The correlation between those results was also examined. The Pearson correlations for Ca and K were 0.9871 and 0.9558, respectively. Method validation using SRM NIST 1548a Typical Diet was also applied. The results showed good agreement between methods; therefore EDXRF method can be used as an alternative method for the determination of Ca and K in food samples.

Development of an analytical procedure for plutonium in the concentration range of femtogram/gram and its application to environmental samples

International Nuclear Information System (INIS)

Schuettelkopf, H.

1981-09-01

To study the behaviour of plutonium in the environment and to measure plutonium in the vicinity of nuclear facilities, a quick, sensitive analytical method is required which can be applied to all sample materials found in the environment. For a sediment contaminated with plutonium a boiling out method using first HNO 3 /HF and subsequently HNO 3 /Al(NO 3 ) 3 was found to be successful. The leaching solution was then extracted by TOPO and the plutonium backextracted by ascorbic acid/HCl. Some different purification steps and finally electroplating using ammonium oxalate led to an optimum sample for α- spectroscopic determination of plutonium. An analytical method was worked out for plutonium which can be applied to all materials found in the environment. The sample size is 100 g but it might also be much greater. The average chemical yield is 70 and 80%. The detection limit for soil samples is 0.1 fCi/g and for plant samples 0.5 fCi/g. One technician can perform eight analyses per working day. The analytical procedure was applied to a large number of environmental samples and the results of these analyses are indicated. (orig./RB) [de

Analytical results and sample locality map for rock, stream-sediment, and soil samples, Northern and Eastern Coloado Desert BLM Resource Area, Imperial, Riverside, and San Bernardino Counties, California

Science.gov (United States)

King, Harley D.; Chaffee, Maurice A.

2000-01-01

INTRODUCTION In 1996-1998 the U.S. Geological Survey (USGS) conducted a geochemical study of the Bureau of Land Management's (BLM) 5.5 million-acre Northern and Eastern Colorado Desert Resource Area (usually referred to as the NECD in this report), Imperial, Riverside, and San Bernardino Counties, southeastern California (figure 1). This study was done in support of the BLM's Coordinated Management Plan for the area. This report presents analytical data from this study. To provide comprehensive coverage of the NECD, we compiled and examined all available geochemical data, in digital form, from previous studies in the area, and made sample-site plots to aid in determining where sample-site coverage and analyses were sufficient, which samples should be re-analyzed, and where additional sampling was needed. Previous investigations conducted in parts of the current study area included the National Uranium Resource Evaluation (NURE) program studies of the Needles and Salton Sea 1? x 2? quadrangles; USGS studies of 12 BLM Wilderness Study Areas (WSAs) (Big Maria Mountains, Chemehuevi Mountains, Chuckwalla Mountains, Coxcomb Mountains, Mecca Hills, Orocopia Mountains, Palen-McCoy, Picacho Peak, Riverside Mountains, Sheephole Valley (also known as Sheep Hole/Cadiz), Turtle Mountains, and Whipple Mountains); and USGS studies in the Needles and El Centro 1? x 2? quadrangles done during the early 1990s as part of a project to identify the regional geochemistry of southern California. Areas where we did new sampling of rocks and stream sediments are mainly in the Chocolate Mountain Aerial Gunnery Range and in Joshua Tree National Park, which extends into the west-central part of the NECD, as shown in figure 1 and figure 2. This report contains analytical data for 132 rock samples and 1,245 stream-sediment samples collected by the USGS, and 362 stream-sediment samples and 189 soil samples collected during the NURE program. All samples are from the Northern and Eastern Colorado

Final Report on the Analytical Results for Tank Farm Samples in Support of Salt Dissolution Evaluation

International Nuclear Information System (INIS)

Hobbs, D.T.

1996-01-01

Recent processing of dilute solutions through the 2H-Evaporator system caused dissolution of salt in Tank 38H, the concentrate receipt tank. This report documents analytical results for samples taken from this evaporator system

Experience-Sampling Methodology with a Mobile Device in Fibromyalgia

Directory of Open Access Journals (Sweden)

Castilla Diana

2012-01-01

Full Text Available This work describes the usability studies conducted in the development of an experience-sampling methodology (ESM system running in a mobile device. The goal of the system is to improve the accuracy and ecology in gathering daily self-report data in individuals suffering a chronic pain condition, fibromyalgia. The usability studies showed that the developed software to conduct ESM with mobile devices (smartphones, cell phones can be successfully used by individuals with fibromyalgia of different ages and with low level of expertise in the use of information and communication technologies. 100% of users completed the tasks successfully, although some have completely illiterate. Also there seems to be a clear difference in the way of interaction obtained in the two studies carried out.

Recent bibliography on analytical and sampling problems of a PWR primary coolant Suppl. 3

International Nuclear Information System (INIS)

Illy, H.

1985-03-01

The present supplement to the bibliography on analytical and sampling problems of PWR primary coolant covers the literature published in 1984 and includes some references overlooked in the previous volumes dealing with the publications of the last 10 years. References are devided into topics characterized by the following headlines: boric acid; chloride; chlorine; carbon dioxide; general; gas analysis; hydrogen isotopes; iodine; iodide; nitrogen; noble gases and radium; ammonia; ammonium; oxygen; other elements; radiation monitoring; reactor safety; sampling; water chemistry. Under a given subject bibliographical information is listed in alphabetical order of the authors. (V.N.)

Microgenetic Learning Analytics Methods: Workshop Report

Science.gov (United States)

Aghababyan, Ani; Martin, Taylor; Janisiewicz, Philip; Close, Kevin

2016-01-01

Learning analytics is an emerging discipline and, as such, benefits from new tools and methodological approaches. This work reviews and summarizes our workshop on microgenetic data analysis techniques using R, held at the second annual Learning Analytics Summer Institute in Cambridge, Massachusetts, on 30 June 2014. Specifically, this paper…

Studies on the spectral interference of gadolinium on different analytes in inductively coupled plasma atomic emission spectroscopy

International Nuclear Information System (INIS)

Sengupta, Arijit; Thulasidas, S.K.; Natarajan, V.; Airan, Yougant

2015-01-01

Due to the multi-electronic nature, rare earth elements are prone to exhibit spectral interference in ICP-AES, which leads to erroneous determination of analytes in presence of such matrix. This interference is very significant, when the analytes are to be determined at trace level in presence of emission rich matrix elements. An attempt was made to understand the spectral interference of Gd on 29 common analytes like Ag, Al, B, Ba, Bi, Ca, Cd, Ce, Co, Cr, Cu, Dy, Fe, Ga, Gd, In, La, Li, Lu, Mg, Mn, Na, Nd, Ni, Pb, Pr, Sr, Tl and Zn using ICP-AES with capacitive Charged Coupled Device (CCD) as detector. The present study includes identification of suitable interference free analytical lines of these analytes, evaluation of correction factor for each analytical line and determination of tolerance levels of these analytical lines along with the ICP-AES based methodology for simultaneous determination of Gd. Based on the spectral interference study, an ICP-AES based method was developed for the determination of these analytes at trace level in presence of Gd matrix without chemical separation. Further the developed methodology was validated using synthetic samples prepared from commercially available reference material solution of individual element; the results were found to be satisfactory. The method was also compared with other existing techniques

Current status of JAERI program on development of ultra-trace-analytical technology for safeguards environmental samples

International Nuclear Information System (INIS)

Adachi, T.; Usuda, S.; Watanabe, K.

2001-01-01

Full text: In order to contribute to the strengthened safeguards system based on the Program 93+2 of the IAEA, Japan Atomic Energy Research Institute (JAERI) is developing analytical technology for ultra-trace amounts of nuclear materials in environmental samples, and constructed the CLEAR facility (Clean Laboratory for Environmental Analysis and Research) for this purpose. The development of the technology is carried out, at existing laboratories for time being, in the following fields: screening, bulk analysis and particle analysis. The screening aims at estimating the amounts of nuclear materials in environmental samples to be introduced into the clean rooms, and is the first step to avoid cross-contamination among the samples and contamination of the clean rooms themselves. In addition to ordinary radiation spectrometry, Compton suppression technique was applied to low energy γ- and X-ray measurements, and sufficient reduction in background level has been demonstrated. Another technique in examination is imaging-plate method, which is a kind of autoradiography and suitable for determination of radioactive-particle distribution in the samples as well as for semiquantitative determination. As for the bulk analysis, the efforts are temporally made on uranium in swipe samples. Preliminary examination for optimization of sample pre-treatment conditions is in progress. At present, ashing by low-temperature-plasma method gives better results than high-temperature ashing or acid leaching. For the isotopic ratio measurement, instrumental performance of inductively-coupled plasma mass spectrometry (ICP-MS) are mainly examined because sample preparation for ICP-MS is simpler than that for thermal ionization mass spectrometry (TIMS). It was found by our measurement that the swipe material (TexWipe TX304, usually used by IAEA) contains un-negligible uranium blank with large deviation (2-6 ng/sheet). This would introduce significant uncertainty in the trace analysis. JAERI

Measuring myokines with cardiovascular functions: pre-analytical variables affecting the analytical output.

Science.gov (United States)

Lombardi, Giovanni; Sansoni, Veronica; Banfi, Giuseppe

2017-08-01

In the last few years, a growing number of molecules have been associated to an endocrine function of the skeletal muscle. Circulating myokine levels, in turn, have been associated with several pathophysiological conditions including the cardiovascular ones. However, data from different studies are often not completely comparable or even discordant. This would be due, at least in part, to the whole set of situations related to the preparation of the patient prior to blood sampling, blood sampling procedure, processing and/or store. This entire process constitutes the pre-analytical phase. The importance of the pre-analytical phase is often not considered. However, in routine diagnostics, the 70% of the errors are in this phase. Moreover, errors during the pre-analytical phase are carried over in the analytical phase and affects the final output. In research, for example, when samples are collected over a long time and by different laboratories, a standardized procedure for sample collecting and the correct procedure for sample storage are acknowledged. In this review, we discuss the pre-analytical variables potentially affecting the measurement of myokines with cardiovascular functions.

Intermediate algebra & analytic geometry

CERN Document Server

Gondin, William R

1967-01-01

Intermediate Algebra & Analytic Geometry Made Simple focuses on the principles, processes, calculations, and methodologies involved in intermediate algebra and analytic geometry. The publication first offers information on linear equations in two unknowns and variables, functions, and graphs. Discussions focus on graphic interpretations, explicit and implicit functions, first quadrant graphs, variables and functions, determinate and indeterminate systems, independent and dependent equations, and defective and redundant systems. The text then examines quadratic equations in one variable, system

Recommendations for sampling for prevention of hazards in civil defense. On analytics of chemical, biological and radioactive contaminations. Brief instruction for the CBRN (chemical, biological, radioactive, nuclear) sampling

International Nuclear Information System (INIS)

Bachmann, Udo; Biederbick, Walter; Derakshani, Nahid

2010-01-01

The recommendation for sampling for prevention of hazards in civil defense is describing the analytics of chemical, biological and radioactive contaminations and includes detail information on the sampling, protocol preparation and documentation procedures. The volume includes a separate brief instruction for the CBRN (chemical, biological, radioactive, nuclear) sampling.

Concrete crushing and sampling, a methodology and technology for the unconditional release of concrete material from decommissioning

International Nuclear Information System (INIS)

Baumann, S.; Teunckens, L.; Walthery, R.; Lewandowski, P.; Millen, D.

2002-01-01

Belgoprocess started the industrial decommissioning of the main process building of the former Eurochemic reprocessing plant in 1990, after completion of a pilot project. Two small storage buildings for final products from reprocessing were dismantled to verify the assumptions made in a previous paper study on decommissioning, to demonstrate and develop dismantling techniques and to train personnel. Both buildings were emptied and decontaminated to background levels. They were demolished and the remaining concrete debris was disposed of as industrial waste and green field conditions restored. Currently, the decommissioning operations carried out at the main building have made substantial progress. They are executed on an industrial scale and will continue till the end of 2005. In view of the final demolition of the building, a clearance methodology has to be proposed. Application of the methodology applied for the storage buildings of the pilot project is complicated for several reasons. Although this methodology is not rejected as such, an alternative has been studied thoroughly. It considers at least one complete measurement of all concrete structures and the removal of all detected residual radioactivity. This monitoring sequence is followed by a controlled demolition of the concrete structures and crushing of the resulting concrete parts to smaller particles. During the crushing operations, metal parts are separated from the concrete and representative concrete samples are taken. The frequency of sampling meets the prevailing standards. In a further step, the concrete samples are milled, homogenised, and a smaller fraction is sent to the laboratory for analyses. The paper describes the developed concrete crushing and sampling methodology. (authors)

Optimized Analytical Method to Determine Gallic and Picric Acids in Pyrotechnic Samples by Using HPLC/UV (Reverse Phase)

International Nuclear Information System (INIS)

Garcia Alonso, S.; Perez Pastor, R. M.

2013-01-01

A study on the optimization and development of a chromatographic method for the determination of gallic and picric acids in pyrotechnic samples is presented. In order to achieve this, both analytical conditions by HPLC with diode detection and extraction step of a selected sample were studied. (Author)

Analytic escrutineo for plaguicidas organofosforados in blood in forensic cases by means of SPME-GC/NPD

International Nuclear Information System (INIS)

Fernandez Quesada, K.; Saenz Ugalde, M. F.

2003-01-01

The plaguicidas organophosphorus represent one of the most important causes of intoxication in Costa Rica; 20% of the cases received in the Section of Toxicology of the Department of Forensic Sciences of the Organism of Judicial Investigation (OIJ) are related to these plaguicidas. At the present time, the employed techniques in this institution to carry out the organophosphorus analyses in blood, present important limitations in their analytic potential. As a consequence, it is necessary to look for new methodologies, with the purpose to obtain a great specificity, and to diminish the limits of detection. This would allow a more qualified service that assures the validity and reliability of the results. Besides, it is an ideal instrument for the correct administration of justice of the Judicial Authorities. In this final work of graduation, it develops a methodology for the scrutiny of pesticides organophosphorus, in which a sample of biological origin of forensic importance is used. This employs a technique of quick, simple and clean extraction, using a separation method of detection of high analytic sensibility. In the methodology's development, samples of total blood, and the microextraccion techniques in solid phase will be used (SPME), and detection with gas chromatography by a specific instrumental detector of match and nitrogen (GCINPD) [es

Defining And Characterizing Sample Representativeness For DWPF Melter Feed Samples

Energy Technology Data Exchange (ETDEWEB)

Shine, E. P.; Poirier, M. R.

2013-10-29

Representative sampling is important throughout the Defense Waste Processing Facility (DWPF) process, and the demonstrated success of the DWPF process to achieve glass product quality over the past two decades is a direct result of the quality of information obtained from the process. The objective of this report was to present sampling methods that the Savannah River Site (SRS) used to qualify waste being dispositioned at the DWPF. The goal was to emphasize the methodology, not a list of outcomes from those studies. This methodology includes proven methods for taking representative samples, the use of controlled analytical methods, and data interpretation and reporting that considers the uncertainty of all error sources. Numerous sampling studies were conducted during the development of the DWPF process and still continue to be performed in order to evaluate options for process improvement. Study designs were based on use of statistical tools applicable to the determination of uncertainties associated with the data needs. Successful designs are apt to be repeated, so this report chose only to include prototypic case studies that typify the characteristics of frequently used designs. Case studies have been presented for studying in-tank homogeneity, evaluating the suitability of sampler systems, determining factors that affect mixing and sampling, comparing the final waste glass product chemical composition and durability to that of the glass pour stream sample and other samples from process vessels, and assessing the uniformity of the chemical composition in the waste glass product. Many of these studies efficiently addressed more than one of these areas of concern associated with demonstrating sample representativeness and provide examples of statistical tools in use for DWPF. The time when many of these designs were implemented was in an age when the sampling ideas of Pierre Gy were not as widespread as they are today. Nonetheless, the engineers and

Defining And Characterizing Sample Representativeness For DWPF Melter Feed Samples

International Nuclear Information System (INIS)

Shine, E. P.; Poirier, M. R.

2013-01-01

Representative sampling is important throughout the Defense Waste Processing Facility (DWPF) process, and the demonstrated success of the DWPF process to achieve glass product quality over the past two decades is a direct result of the quality of information obtained from the process. The objective of this report was to present sampling methods that the Savannah River Site (SRS) used to qualify waste being dispositioned at the DWPF. The goal was to emphasize the methodology, not a list of outcomes from those studies. This methodology includes proven methods for taking representative samples, the use of controlled analytical methods, and data interpretation and reporting that considers the uncertainty of all error sources. Numerous sampling studies were conducted during the development of the DWPF process and still continue to be performed in order to evaluate options for process improvement. Study designs were based on use of statistical tools applicable to the determination of uncertainties associated with the data needs. Successful designs are apt to be repeated, so this report chose only to include prototypic case studies that typify the characteristics of frequently used designs. Case studies have been presented for studying in-tank homogeneity, evaluating the suitability of sampler systems, determining factors that affect mixing and sampling, comparing the final waste glass product chemical composition and durability to that of the glass pour stream sample and other samples from process vessels, and assessing the uniformity of the chemical composition in the waste glass product. Many of these studies efficiently addressed more than one of these areas of concern associated with demonstrating sample representativeness and provide examples of statistical tools in use for DWPF. The time when many of these designs were implemented was in an age when the sampling ideas of Pierre Gy were not as widespread as they are today. Nonetheless, the engineers and

Methodological issues affecting the study of fish parasites. II. Sampling method affects ectoparasite studies

Czech Academy of Sciences Publication Activity Database

Kvach, Yuriy; Ondračková, Markéta; Janáč, Michal; Jurajda, Pavel

2016-01-01

Roč. 121, č. 1 (2016), s. 59-66 ISSN 0177-5103 R&D Projects: GA ČR GBP505/12/G112 Institutional support: RVO:68081766 Keywords : Parasite community * Fish sampling method * Methodology * Parasitological examination * Rutilus rutilus Subject RIV: EG - Zoology Impact factor: 1.549, year: 2016

Arsenic speciation in marine organisms: from the analytical methodology to the constitution of reference materials

Energy Technology Data Exchange (ETDEWEB)

El Moll, A. [Laboratoire de Chimie Minerale et Analytique, URA 405 du CNRS, E. H. I. C. S., 1 rue Blaise Pascal, F-67008 Strasbourg Cedex (France); Heimburger, R. [Laboratoire de Chimie Minerale et Analytique, URA 405 du CNRS, E. H. I. C. S., 1 rue Blaise Pascal, F-67008 Strasbourg Cedex (France); Lagarde, F. [Laboratoire de Chimie Minerale et Analytique, URA 405 du CNRS, E. H. I. C. S., 1 rue Blaise Pascal, F-67008 Strasbourg Cedex (France); Leroy, M.J.F. [Laboratoire de Chimie Minerale et Analytique, URA 405 du CNRS, E. H. I. C. S., 1 rue Blaise Pascal, F-67008 Strasbourg Cedex (France); Maier, E. [Commission of the European Communities, Measurements and Testing Programme (BCR), 75 rue Montoyer, B-1049 Brussels (Belgium)

1996-03-01

An analytical procedure for total arsenic and arsenic species quantification in marine organisms has been developed. Fresh materials are freeze-dried and reduced to powders before analysis. Arsenic is determined either by energy dispersive X-ray fluorescence (EDXRF) directly or by inductively coupled plasma optical emission spectrometry (ICP/OES) after microwave digestion. Arsenic speciation is performed on the extracted sample using liquid chromatography coupled to ICP/OES for arsenobetaine and arsenocholine determination and to the hydride generation-quartz furnace atomic absorption spectrometric technique for arsenite, arsenate, monomethylarsonic and dimethylarsinic acids quantification. Special precautions are taken to avoid losses or contaminations as well as to prevent analytical errors during the quantification stage. Other methods are applied and the corresponding results compared for each step of the procedure. The method is finally validated by means of intercomparison studies within the Measurements and Testing Programme of the European Community (formely BCR). (orig.). With 9 figs., 5 tabs.

Evaluation of analytical results on DOE Quality Assessment Program Samples

International Nuclear Information System (INIS)

Jaquish, R.E.; Kinnison, R.R.; Mathur, S.P.; Sastry, R.

1985-01-01

Criteria were developed for evaluating the participants analytical results in the DOE Quality Assessment Program (QAP). Historical data from previous QAP studies were analyzed using descriptive statistical methods to determine the interlaboratory precision that had been attained. Performance criteria used in other similar programs were also reviewed. Using these data, precision values and control limits were recommended for each type of analysis performed in the QA program. Results of the analysis performed by the QAP participants on the November 1983 samples were statistically analyzed and evaluated. The Environmental Measurements Laboratory (EML) values were used as the known values and 3-sigma precision values were used as control limits. Results were submitted by 26 participating laboratories for 49 different radionuclide media combinations. The participants reported 419 results and of these, 350 or 84% were within control limits. Special attention was given to the data from gamma spectral analysis of air filters and water samples. both normal probability and box plots were prepared for each nuclide to help evaluate the distribution of the data. Results that were outside the expected range were identified and suggestions made that laboratories check calculations, and procedures on these results

Stability of purgeable VOCs in water samples during pre-analytical holding: Part 1, Analysis by a commercial laboratory

Energy Technology Data Exchange (ETDEWEB)

West, O.R.; Bayne, C.K.; Siegrist, R.L.; Holden, W.L.; Scarborough, S.S. [Oak Ridge National Lab., TN (United States); Bottrell, D.W. [USDOE, Washington, DC (United States)

1996-10-01

This study was undertaken to examine the hypothesis that prevalent and priority purgeable VOCs in properly preserved water samples are stable for at least 28 days. (VOCs are considered stable if concentrations do not change by more than 10%.) Surface water was spiked with 44 purgeable VOCs. Results showed that the measurement of 35 out of 44 purgeable VOCs in properly preserved water samples (4 C, 250 mg NaHSO{sub 4}, no headspace in 40 mL VOC vials with 0.010-in. Teflon-lined silicone septum caps) will not be affected by sample storage for 28 days. Larger changes (>10%) and low practical reporting times were observed for a few analytes, e.g. acrolein, CS{sub 2}, vinyl acetate, etc.; these also involve other analytical problems. Advantages of a 28-day (compared to 14-day) holding time are pointed out.

User's and reference guide to the INEL RML/analytical radiochemistry sample tracking database version 1.00

International Nuclear Information System (INIS)

Femec, D.A.

1995-09-01

This report discusses the sample tracking database in use at the Idaho National Engineering Laboratory (INEL) by the Radiation Measurements Laboratory (RML) and Analytical Radiochemistry. The database was designed in-house to meet the specific needs of the RML and Analytical Radiochemistry. The report consists of two parts, a user's guide and a reference guide. The user's guide presents some of the fundamentals needed by anyone who will be using the database via its user interface. The reference guide describes the design of both the database and the user interface. Briefly mentioned in the reference guide are the code-generating tools, CREATE-SCHEMA and BUILD-SCREEN, written to automatically generate code for the database and its user interface. The appendices contain the input files used by the these tools to create code for the sample tracking database. The output files generated by these tools are also included in the appendices

Glycan characterization of the NIST RM monoclonal antibody using a total analytical solution: From sample preparation to data analysis.

Science.gov (United States)

Hilliard, Mark; Alley, William R; McManus, Ciara A; Yu, Ying Qing; Hallinan, Sinead; Gebler, John; Rudd, Pauline M

Glycosylation is an important attribute of biopharmaceutical products to monitor from development through production. However, glycosylation analysis has traditionally been a time-consuming process with long sample preparation protocols and manual interpretation of the data. To address the challenges associated with glycan analysis, we developed a streamlined analytical solution that covers the entire process from sample preparation to data analysis. In this communication, we describe the complete analytical solution that begins with a simplified and fast N-linked glycan sample preparation protocol that can be completed in less than 1 hr. The sample preparation includes labelling with RapiFluor-MS tag to improve both fluorescence (FLR) and mass spectral (MS) sensitivities. Following HILIC-UPLC/FLR/MS analyses, the data are processed and a library search based on glucose units has been included to expedite the task of structural assignment. We then applied this total analytical solution to characterize the glycosylation of the NIST Reference Material mAb 8761. For this glycoprotein, we confidently identified 35 N-linked glycans and all three major classes, high mannose, complex, and hybrid, were present. The majority of the glycans were neutral and fucosylated; glycans featuring N-glycolylneuraminic acid and those with two galactoses connected via an α1,3-linkage were also identified.

Recent bibliography on analytical and sampling problems of a PWR primary coolant Pt. 1

International Nuclear Information System (INIS)

Illy, H.

1981-12-01

The first bibliography on analytical and sampling problems of a PWR primary coolant (KFKI Report-1980-48) was published in 1980 and it covered the literature published in the previous 8-10 years. The present supplement reviews the subsequent literature up till December 1981. It also includes some references overlooked in the first volume. The serial numbers are continued from the first bibliography. (author)

Abundance, distribution and diversity of gelatinous predators along the northern Mid-Atlantic Ridge: A comparison of different sampling methodologies.

Directory of Open Access Journals (Sweden)

Aino Hosia

Full Text Available The diversity and distribution of gelatinous zooplankton were investigated along the northern Mid-Atlantic Ridge (MAR from June to August 2004.Here, we present results from macrozooplankton trawl sampling, as well as comparisons made between five different methodologies that were employed during the MAR-ECO survey. In total, 16 species of hydromedusae, 31 species of siphonophores and four species of scyphozoans were identified to species level from macrozooplankton trawl samples. Additional taxa were identified to higher taxonomic levels and a single ctenophore genus was observed. Samples were collected at 17 stations along the MAR between the Azores and Iceland. A divergence in the species assemblages was observed at the southern limit of the Subpolar Frontal Zone. The catch composition of gelatinous zooplankton is compared between different sampling methodologies including: a macrozooplankton trawl; a Multinet; a ringnet attached to bottom trawl; and optical platforms (Underwater Video Profiler (UVP & Remotely Operated Vehicle (ROV. Different sampling methodologies are shown to exhibit selectivity towards different groups of gelatinous zooplankton. Only ~21% of taxa caught during the survey were caught by both the macrozooplankton trawl and the Multinet when deployed at the same station. The estimates of gelatinous zooplankton abundance calculated using these two gear types also varied widely (1.4 ± 0.9 individuals 1000 m-3 estimated by the macrozooplankton trawl vs. 468.3 ± 315.4 individuals 1000 m-3 estimated by the Multinet (mean ± s.d. when used at the same stations (n = 6. While it appears that traditional net sampling can generate useful data on pelagic cnidarians, comparisons with results from the optical platforms suggest that ctenophore diversity and abundance are consistently underestimated, particularly when net sampling is conducted in combination with formalin fixation. The results emphasise the importance of considering

Abundance, distribution and diversity of gelatinous predators along the northern Mid-Atlantic Ridge: A comparison of different sampling methodologies

Science.gov (United States)

Falkenhaug, Tone; Baxter, Emily J.

2017-01-01

The diversity and distribution of gelatinous zooplankton were investigated along the northern Mid-Atlantic Ridge (MAR) from June to August 2004.Here, we present results from macrozooplankton trawl sampling, as well as comparisons made between five different methodologies that were employed during the MAR-ECO survey. In total, 16 species of hydromedusae, 31 species of siphonophores and four species of scyphozoans were identified to species level from macrozooplankton trawl samples. Additional taxa were identified to higher taxonomic levels and a single ctenophore genus was observed. Samples were collected at 17 stations along the MAR between the Azores and Iceland. A divergence in the species assemblages was observed at the southern limit of the Subpolar Frontal Zone. The catch composition of gelatinous zooplankton is compared between different sampling methodologies including: a macrozooplankton trawl; a Multinet; a ringnet attached to bottom trawl; and optical platforms (Underwater Video Profiler (UVP) & Remotely Operated Vehicle (ROV)). Different sampling methodologies are shown to exhibit selectivity towards different groups of gelatinous zooplankton. Only ~21% of taxa caught during the survey were caught by both the macrozooplankton trawl and the Multinet when deployed at the same station. The estimates of gelatinous zooplankton abundance calculated using these two gear types also varied widely (1.4 ± 0.9 individuals 1000 m-3 estimated by the macrozooplankton trawl vs. 468.3 ± 315.4 individuals 1000 m-3 estimated by the Multinet (mean ± s.d.) when used at the same stations (n = 6). While it appears that traditional net sampling can generate useful data on pelagic cnidarians, comparisons with results from the optical platforms suggest that ctenophore diversity and abundance are consistently underestimated, particularly when net sampling is conducted in combination with formalin fixation. The results emphasise the importance of considering sampling methodology

Abundance, distribution and diversity of gelatinous predators along the northern Mid-Atlantic Ridge: A comparison of different sampling methodologies.

Science.gov (United States)

Hosia, Aino; Falkenhaug, Tone; Baxter, Emily J; Pagès, Francesc

2017-01-01

The diversity and distribution of gelatinous zooplankton were investigated along the northern Mid-Atlantic Ridge (MAR) from June to August 2004.Here, we present results from macrozooplankton trawl sampling, as well as comparisons made between five different methodologies that were employed during the MAR-ECO survey. In total, 16 species of hydromedusae, 31 species of siphonophores and four species of scyphozoans were identified to species level from macrozooplankton trawl samples. Additional taxa were identified to higher taxonomic levels and a single ctenophore genus was observed. Samples were collected at 17 stations along the MAR between the Azores and Iceland. A divergence in the species assemblages was observed at the southern limit of the Subpolar Frontal Zone. The catch composition of gelatinous zooplankton is compared between different sampling methodologies including: a macrozooplankton trawl; a Multinet; a ringnet attached to bottom trawl; and optical platforms (Underwater Video Profiler (UVP) & Remotely Operated Vehicle (ROV)). Different sampling methodologies are shown to exhibit selectivity towards different groups of gelatinous zooplankton. Only ~21% of taxa caught during the survey were caught by both the macrozooplankton trawl and the Multinet when deployed at the same station. The estimates of gelatinous zooplankton abundance calculated using these two gear types also varied widely (1.4 ± 0.9 individuals 1000 m-3 estimated by the macrozooplankton trawl vs. 468.3 ± 315.4 individuals 1000 m-3 estimated by the Multinet (mean ± s.d.) when used at the same stations (n = 6). While it appears that traditional net sampling can generate useful data on pelagic cnidarians, comparisons with results from the optical platforms suggest that ctenophore diversity and abundance are consistently underestimated, particularly when net sampling is conducted in combination with formalin fixation. The results emphasise the importance of considering sampling methodology

Historical review of transuranic analytical methodology

International Nuclear Information System (INIS)

Wessman, R.A.; Leventhal, L.

1977-01-01

The methods used for the analysis of the transuranic elements neptunium, plutonium, americium, and curium are reviewed. Particular attention is given to those procedures suitable for low-level environmental and biological assessment. The preparation of such samples, derived from a variety of sources and incorporated in different masses and volumes of soils, water, vegetation, and biological matrices, is described. A comprehensive discussion of matrix dissolution and equilibration techniques indicates that complete dissolution employing tracer techniques is to be preferred. Leaching of large soil samples is satisfactory for worldwide fallout. Individual and sequential separation and purification procedures, including precipitation, extraction, and ion exchange methods, are described. Sample preparation techniques for radiometric assay, such as stippling, evaporation, and plating, are reviewed. For both tracer and nuclide assay, electroplating provides the thin samples suitable for alpha pulse height analysis. Past and current counting methods for the transuranic alpha, beta, and gamma emitters are reviewed

Methodology for Isolation, Identification and Characterization of Microvesicles in Peripheral Blood

Science.gov (United States)

Jayachandran, Muthuvel; Miller, Virginia M.; Heit, John A.; Owen, Whyte G.

2011-01-01

Rationale Analyses of circulating cell membrane-derived microvesicles (MV) have come under scrutiny as potential diagnostic and prognostic biomarkers of disease. However, methods to isolate, label and quantify MV have been neither systematized nor validated. Objective To determine how pre-analytical, analytical and post-analytical factors affect plasma MV counts, markers for cell of origin and expression of procoagulant surface phosphatidylserine. Methods and Results Peripheral venous blood samples were collected from healthy volunteers and patients with cardiovascular disease and/or diabetes. Effects of blood sample collection, anticoagulant and sample processing to platelet free plasma (PFP), and MV isolation, staining and storage (freeze-thaw) and cytometer design were evaluated with replicate samples from these populations. The key finding is that use of citrate or EDTA anticoagulants decreases or eliminates microvesicles from plasma by inducing adhesion of the microvesicles to platelets or other formed elements. Protease inhibitor anticoagulants, including heparin, preserve MV counts. A centrifugation protocol was developed in which recovery of isolated MV was high with resolution down to the equivalent light scatter of 0.2 micron latex beads. Each procedure was systematically evaluated for its impact on the MV counts and characteristics. Conclusion This study provides a systematic methodology for MV isolation, identification and quantification, essential for development of MV as diagnostic and prognostic biomarkers of disease. PMID:22075275

Information-analytical maintenance of AIC at regional level

OpenAIRE

MOYSEENKO I.P.

2013-01-01

Submitted approaches to system information and analytical support regional management. Formulated methodology of information and analytical support regional agribusiness management with regard to models of EHS and security settings. Describe the nature and function of monitoring objects of study.

Methodological effects in Fourier transform infrared (FTIR) spectroscopy: Implications for structural analyses of biomacromolecular samples

Science.gov (United States)

Kamnev, Alexander A.; Tugarova, Anna V.; Dyatlova, Yulia A.; Tarantilis, Petros A.; Grigoryeva, Olga P.; Fainleib, Alexander M.; De Luca, Stefania

2018-03-01

A set of experimental data obtained by Fourier transform infrared (FTIR) spectroscopy (involving the use of samples ground and pressed with KBr, i.e. in a polar halide matrix) and by matrix-free transmission FTIR or diffuse reflectance infrared Fourier transform (DRIFT) spectroscopic methodologies (involving measurements of thin films or pure powdered samples, respectively) were compared for several different biomacromolecular substances. The samples under study included poly-3-hydroxybutyrate (PHB) isolated from cell biomass of the rhizobacterium Azospirillum brasilense; dry PHB-containing A. brasilense biomass; pectin (natural carboxylated heteropolysaccharide of plant origin; obtained from apple peel) as well as its chemically modified derivatives obtained by partial esterification of its galacturonide-chain hydroxyl moieties with palmitic, oleic and linoleic acids. Significant shifts of some FTIR vibrational bands related to polar functional groups of all the biomacromolecules under study, induced by the halide matrix used for preparing the samples for spectroscopic measurements, were shown and discussed. A polar halide matrix used for preparing samples for FTIR measurements was shown to be likely to affect band positions not only per se, by affecting band energies or via ion exchange (e.g., with carboxylate moieties), but also by inducing crystallisation of metastable amorphous biopolymers (e.g., PHB of microbial origin). The results obtained have important implications for correct structural analyses of polar, H-bonded and/or amphiphilic biomacromolecular systems using different methodologies of FTIR spectroscopy.

Sampling and analysis plan for the 100-D Ponds voluntary remediation project

International Nuclear Information System (INIS)

1996-08-01

This Sampling and Analysis Plan (SAP) describes the sampling and analytical activities which will be performed to support closure of the 100-D Ponds Resource Conservation and Recovery Act (RCRA) treatment, storage, and/or disposal (TSD) unit. This SAP includes the Field Sampling Plan (FSP) presented in Section 2.0, and the Quality Assurance Project Plan (QAPjP) described in Section 3.0. The FSP defines the sampling and analytical methodologies to be performed, and the QAPjP provides or includes information on the requirements for precision, accuracy, representativeness, comparability, and completeness of the analytical data. This sampling and analysis plan was developed using the Environmental Protection Agency's Seven-Step Data Quality Objectives (DQO) Guidance (EPA, 1994). The purpose of the DQO meetings was (1) to identify the contaminants of concern and their cleanup levels under the Washington State Model Toxics Control Act (MTCA, WAC-173-340) Method B, and (2) to determine the number and locations of samples necessary to verify that the 100-D Ponds meet the cleanup criteria. The data collected will be used to support RCRA closure of this TSD unit

Analytical Method to Estimate the Complex Permittivity of Oil Samples

Directory of Open Access Journals (Sweden)

Lijuan Su

2018-03-01

Full Text Available In this paper, an analytical method to estimate the complex dielectric constant of liquids is presented. The method is based on the measurement of the transmission coefficient in an embedded microstrip line loaded with a complementary split ring resonator (CSRR, which is etched in the ground plane. From this response, the dielectric constant and loss tangent of the liquid under test (LUT can be extracted, provided that the CSRR is surrounded by such LUT, and the liquid level extends beyond the region where the electromagnetic fields generated by the CSRR are present. For that purpose, a liquid container acting as a pool is added to the structure. The main advantage of this method, which is validated from the measurement of the complex dielectric constant of olive and castor oil, is that reference samples for calibration are not required.

Optimisation (sampling strategies and analytical procedures) for site specific environment monitoring at the areas of uranium production legacy sites in Ukraine - 59045

International Nuclear Information System (INIS)

Voitsekhovych, Oleg V.; Lavrova, Tatiana V.; Kostezh, Alexander B.

2012-01-01

There are many sites in the world, where Environment are still under influence of the contamination related to the Uranium production carried out in past. Author's experience shows that lack of site characterization data, incomplete or unreliable environment monitoring studies can significantly limit quality of Safety Assessment procedures and Priority actions analyses needed for Remediation Planning. During recent decades the analytical laboratories of the many enterprises, currently being responsible for establishing the site specific environment monitoring program have been significantly improved their technical sampling and analytical capacities. However, lack of experience in the optimal site specific sampling strategy planning and also not enough experience in application of the required analytical techniques, such as modern alpha-beta radiometers, gamma and alpha spectrometry and liquid-scintillation analytical methods application for determination of U-Th series radionuclides in the environment, does not allow to these laboratories to develop and conduct efficiently the monitoring programs as a basis for further Safety Assessment in decision making procedures. This paper gives some conclusions, which were gained from the experience establishing monitoring programs in Ukraine and also propose some practical steps on optimization in sampling strategy planning and analytical procedures to be applied for the area required Safety assessment and justification for its potential remediation and safe management. (authors)

Sample handling in surface sensitive chemical and biological sensing: a practical review of basic fluidics and analyte transport.

Science.gov (United States)

Orgovan, Norbert; Patko, Daniel; Hos, Csaba; Kurunczi, Sándor; Szabó, Bálint; Ramsden, Jeremy J; Horvath, Robert

2014-09-01

This paper gives an overview of the advantages and associated caveats of the most common sample handling methods in surface-sensitive chemical and biological sensing. We summarize the basic theoretical and practical considerations one faces when designing and assembling the fluidic part of the sensor devices. The influence of analyte size, the use of closed and flow-through cuvettes, the importance of flow rate, tubing length and diameter, bubble traps, pressure-driven pumping, cuvette dead volumes, and sample injection systems are all discussed. Typical application areas of particular arrangements are also highlighted, such as the monitoring of cellular adhesion, biomolecule adsorption-desorption and ligand-receptor affinity binding. Our work is a practical review in the sense that for every sample handling arrangement considered we present our own experimental data and critically review our experience with the given arrangement. In the experimental part we focus on sample handling in optical waveguide lightmode spectroscopy (OWLS) measurements, but the present study is equally applicable for other biosensing technologies in which an analyte in solution is captured at a surface and its presence is monitored. Explicit attention is given to features that are expected to play an increasingly decisive role in determining the reliability of (bio)chemical sensing measurements, such as analyte transport to the sensor surface; the distorting influence of dead volumes in the fluidic system; and the appropriate sample handling of cell suspensions (e.g. their quasi-simultaneous deposition). At the appropriate places, biological aspects closely related to fluidics (e.g. cellular mechanotransduction, competitive adsorption, blood flow in veins) are also discussed, particularly with regard to their models used in biosensing. Copyright © 2014 Elsevier B.V. All rights reserved.

Development and implementation of information systems for the DOE's National Analytical Management Program (NAMP)

International Nuclear Information System (INIS)

Streets, W. E.

1999-01-01

The Department of Energy (DOE) faces a challenging environmental management effort, including environmental protection, environmental restoration, waste management, and decommissioning. This effort requires extensive sampling and analysis to determine the type and level of contamination and the appropriate technology for cleanup, and to verify compliance with environmental regulations. Data obtained from these sampling and analysis activities are used to support environmental management decisions. Confidence in the data is critical, having legal, regulatory, and therefore, economic impact. To promote quality in the planning, management, and performance of these sampling and analysis operations, DOE's Office of Environmental Management (EM) has established the National Analytical Management Program (NAMP). With a focus on reducing the estimated costs of over $200M per year for EM's analytical services, NAMP has been charged with developing products that will decrease the costs for DOE complex-wide environmental management while maintaining quality in all aspects of the analytical data generation. As part of this thrust to streamline operations, NAMP is developing centralized information systems that will allow DOE complex personnel to share information about EM contacts at the various sites, pertinent methodologies for environmental restoration and waste management, costs of analyses, and performance of contracted laboratories

Nuclear analytical methods for platinum group elements

International Nuclear Information System (INIS)

2005-04-01

Platinum group elements (PGE) are of special interest for analytical research due to their economic importance like chemical peculiarities as catalysts, medical applications as anticancer drugs, and possible environmental detrimental impact as exhaust from automobile catalyzers. Natural levels of PGE are so low in concentration that most of the current analytical techniques approach their limit of detection capacity. In addition, Ru, Rh, Pd, Re, Os, Ir, and Pt analyses still constitute a challenge in accuracy and precision of quantification in natural matrices. Nuclear analytical techniques, such as neutron activation analysis, X ray fluorescence, or proton-induced X ray emission (PIXE), which are generally considered as reference methods for many analytical problems, are useful as well. However, due to methodological restrictions, they can, in most cases, only be applied after pre-concentration and under special irradiation conditions. This report was prepared following a coordinated research project and a consultants meeting addressing the subject from different viewpoints. The experts involved suggested to discuss the issue according to the (1) application, hence, the concentration levels encountered, and (2) method applied for analysis. Each of the different fields of application needs special consideration for sample preparation, PGE pre-concentration, and determination. Additionally, each analytical method requires special attention regarding the sensitivity and sample type. Quality assurance/quality control aspects are considered towards the end of the report. It is intended to provide the reader of this publication with state-of-the-art information on the various aspects of PGE analysis and to advise which technique might be most suitable for a particular analytical problem related to platinum group elements. In particular, many case studies described in detail from the authors' laboratory experience might help to decide which way to go. As in many cases

Assessment of pesticide contamination in soil samples from an intensive horticulture area, using ultrasonic extraction and gas chromatography-mass spectrometry.

Science.gov (United States)

Gonçalves, C; Alpendurada, M F

2005-03-15

In order to reduce the amount of sample to be collected and the time consumed in the analytical process, a broad range of analytes should be preferably considered in the same analytical procedure. A suitable methodology for pesticide residue analysis in soil samples was developed based on ultrasonic extraction (USE) and gas chromatography-mass spectrometry (GC-MS). For this study, different classes of pesticides were selected, both recent and old persistent molecules: parent compounds and degradation products, namely organochlorine, organophosphorous and pyrethroid insecticides, triazine and acetanilide herbicides and other miscellaneous pesticides. Pesticide residues could be detected in the low- to sub-ppb range (0.05-7.0mugkg(-1)) with good precision (7.5-20.5%, average 13.7% R.S.D.) and extraction efficiency (69-118%, average 88%) for the great majority of analytes. This methodology has been applied in a monitoring program of soil samples from an intensive horticulture area in Póvoa de Varzim, North of Portugal. The pesticides detected in four sampling programs (2001/2002) were the following: lindane, dieldrin, endosulfan, endosulfan sulfate, 4,4'-DDE, 4,4'-DDD, atrazine, desethylatrazine, alachlor, dimethoate, chlorpyrifos, pendimethalin, procymidone and chlorfenvinphos. Pesticide contamination was investigated at three depths and in different soil and crop types to assess the influence of soil characteristics and trends over time.

Sources of pre-analytical variations in yield of DNA extracted from blood samples: analysis of 50,000 DNA samples in EPIC.

Directory of Open Access Journals (Sweden)

Elodie Caboux

Full Text Available The European Prospective Investigation into Cancer and nutrition (EPIC is a long-term, multi-centric prospective study in Europe investigating the relationships between cancer and nutrition. This study has served as a basis for a number of Genome-Wide Association Studies (GWAS and other types of genetic analyses. Over a period of 5 years, 52,256 EPIC DNA samples have been extracted using an automated DNA extraction platform. Here we have evaluated the pre-analytical factors affecting DNA yield, including anthropometric, epidemiological and technical factors such as center of subject recruitment, age, gender, body-mass index, disease case or control status, tobacco consumption, number of aliquots of buffy coat used for DNA extraction, extraction machine or procedure, DNA quantification method, degree of haemolysis and variations in the timing of sample processing. We show that the largest significant variations in DNA yield were observed with degree of haemolysis and with center of subject recruitment. Age, gender, body-mass index, cancer case or control status and tobacco consumption also significantly impacted DNA yield. Feedback from laboratories which have analyzed DNA with different SNP genotyping technologies demonstrate that the vast majority of samples (approximately 88% performed adequately in different types of assays. To our knowledge this study is the largest to date to evaluate the sources of pre-analytical variations in DNA extracted from peripheral leucocytes. The results provide a strong evidence-based rationale for standardized recommendations on blood collection and processing protocols for large-scale genetic studies.

Integrated analytical methodologies for the study of corrosion processes in archaeological bronzes

Energy Technology Data Exchange (ETDEWEB)

Alberghina, Maria Francesca; Barraco, Rosita; Brai, Maria; Schillaci, Tiziano, E-mail: tschillaci@unipa.it; Tranchina, Luigi

2011-02-15

The investigations on structure and micro-chemical composition of archaeological metal alloys are needed in archaeometry. The aim of this study is devoted both to acquire information about their provenance and production technology, and to improve our understanding about the corrosion processes. In this paper we present the study of the corrosion phenomena of bronze samples, laboratory-made according to binary, ternary and quaternary alloys typical of Roman archaeometallurgical production through an integrated methodology based on the use of non or micro invasive physical techniques. Among the analysed samples, two were artificially aged through burial in the archaeological site of Tharros, along the west coast of Sardinia (Italy). The corrosion products, typical of the bronzes in archaeological sites near the sea, have been characterized by non invasive and micro-destructive measurements. In particular, the corrosion patinas were examined through optical microscopy, scanning electron microscopy and microanalysis, X-ray fluorescence and laser ablation spectroscopy. The use of integrated technologies allowed us to determine both the elemental composition and surface morphology of the patina, highlighting the correlation between patina nature and chemical composition of the burial context. Moreover, data obtained by the laser-induced breakdown spectroscopy along the depth profile on the samples, have yielded information about the stratigraphic layers of corrosion products and their growth. Finally, the depth profiles allowed us to verify both the chemical elements constituting the patina, the metal ions constituting the alloy and the occurrence of migration phenomena from bulk to the surface.

Integrated analytical methodologies for the study of corrosion processes in archaeological bronzes

International Nuclear Information System (INIS)

Alberghina, Maria Francesca; Barraco, Rosita; Brai, Maria; Schillaci, Tiziano; Tranchina, Luigi

2011-01-01

The investigations on structure and micro-chemical composition of archaeological metal alloys are needed in archaeometry. The aim of this study is devoted both to acquire information about their provenance and production technology, and to improve our understanding about the corrosion processes. In this paper we present the study of the corrosion phenomena of bronze samples, laboratory-made according to binary, ternary and quaternary alloys typical of Roman archaeometallurgical production through an integrated methodology based on the use of non or micro invasive physical techniques. Among the analysed samples, two were artificially aged through burial in the archaeological site of Tharros, along the west coast of Sardinia (Italy). The corrosion products, typical of the bronzes in archaeological sites near the sea, have been characterized by non invasive and micro-destructive measurements. In particular, the corrosion patinas were examined through optical microscopy, scanning electron microscopy and microanalysis, X-ray fluorescence and laser ablation spectroscopy. The use of integrated technologies allowed us to determine both the elemental composition and surface morphology of the patina, highlighting the correlation between patina nature and chemical composition of the burial context. Moreover, data obtained by the laser-induced breakdown spectroscopy along the depth profile on the samples, have yielded information about the stratigraphic layers of corrosion products and their growth. Finally, the depth profiles allowed us to verify both the chemical elements constituting the patina, the metal ions constituting the alloy and the occurrence of migration phenomena from bulk to the surface.

Use of Hg-Electroplated-Pt Ultramicroelectrode for Determining Elemental Sulphur in Naphtha Samples

Directory of Open Access Journals (Sweden)

Carlos Eduardo de Andrade

2012-01-01

Full Text Available This paper describes the applicability of a Hg-electroplated-Pt ultramicroelectrode in the quantification of elemental sulphur in naphtha samples by square-wave voltammetry. A reproducible deposition methodology was studied and is reported in this paper. This methodology is innovative and relies on the quality of the mercury stock solution to obtain reproducible surfaces required for the analytical methodology. All analyses were performed using a Hg-electroplated-Pt ultramicroelectrode (Hg-Pt UME due to the low sensibility of such devices to ohmic drops in resistive solutions. The responses of the peak areas in voltammetric experiments were linear in all of the range studied. The method developed here is accurate and reproducible, with a detection limit of 0.010 mg L−1 and a good recovery range for both standard solutions of elemental sulphur (85 to 99% and real naphtha sample (79%. These results attest to the potential for the application of this electroanalytical methodology in determining elemental sulphur in naphtha samples containing mercaptans and disulphides.

Analytical and between-subject variation of thrombin generation measured by calibrated automated thrombography on plasma samples.

Science.gov (United States)

Kristensen, Anne F; Kristensen, Søren R; Falkmer, Ursula; Münster, Anna-Marie B; Pedersen, Shona

2018-05-01

The Calibrated Automated Thrombography (CAT) is an in vitro thrombin generation (TG) assay that holds promise as a valuable tool within clinical diagnostics. However, the technique has a considerable analytical variation, and we therefore, investigated the analytical and between-subject variation of CAT systematically. Moreover, we assess the application of an internal standard for normalization to diminish variation. 20 healthy volunteers donated one blood sample which was subsequently centrifuged, aliquoted and stored at -80 °C prior to analysis. The analytical variation was determined on eight runs, where plasma from the same seven volunteers was processed in triplicates, and for the between-subject variation, TG analysis was performed on plasma from all 20 volunteers. The trigger reagents used for the TG assays included both PPP reagent containing 5 pM tissue factor (TF) and PPPlow with 1 pM TF. Plasma, drawn from a single donor, was applied to all plates as an internal standard for each TG analysis, which subsequently was used for normalization. The total analytical variation for TG analysis performed with PPPlow reagent is 3-14% and 9-13% for PPP reagent. This variation can be minimally reduced by using an internal standard but mainly for ETP (endogenous thrombin potential). The between-subject variation is higher when using PPPlow than PPP and this variation is considerable higher than the analytical variation. TG has a rather high inherent analytical variation but considerable lower than the between-subject variation when using PPPlow as reagent.

Radioimmunoassay of h-TSH - methodological suggestions for dealing with medium to large numbers of samples

International Nuclear Information System (INIS)

Mahlstedt, J.

1977-01-01

The article deals with practical aspects of establishing a TSH-RIA for patients, with particular regard to predetermined quality criteria. Methodological suggestions are made for medium to large numbers of samples with the target of reducing monotonous precision working steps by means of simple aids. The quality criteria required are well met, while the test procedure is well adapted to the rhythm of work and may be carried out without loss of precision even with large numbers of samples. (orig.) [de

Methodology for Quantitative Analysis of Large Liquid Samples with Prompt Gamma Neutron Activation Analysis using Am-Be Source

International Nuclear Information System (INIS)

Idiri, Z.; Mazrou, H.; Beddek, S.; Amokrane, A.

2009-01-01

An optimized set-up for prompt gamma neutron activation analysis (PGNAA) with Am-Be source is described and used for large liquid samples analysis. A methodology for quantitative analysis is proposed: it consists on normalizing the prompt gamma count rates with thermal neutron flux measurements carried out with He-3 detector and gamma attenuation factors calculated using MCNP-5. The relative and absolute methods are considered. This methodology is then applied to the determination of cadmium in industrial phosphoric acid. The same sample is then analyzed by inductively coupled plasma (ICP) method. Our results are in good agreement with those obtained with ICP method.

Different methodologies in neutron activation to approach the full analysis of environmental and nutritional samples

International Nuclear Information System (INIS)

Freitas, M.C.; Dionisio, I.; Dung, H.M.

2008-01-01

Different methodologies of neutron activation analysis (NAA) are now available at the Technological and Nuclear Institute (Sacavem, Portugal), namely Compton suppression, epithermal activation, replicate and cyclic activation, and low energy photon measurement. Prompt gamma activation analysis (PGAA) will be implemented soon. Results by instrumental NAA and PGAA on environmental and nutritional samples are discussed herein, showing that PGAA - carried out at the Institute of Isotope Research (Budapest, Hungary) - brings about an effective input to assessing relevant elements. Sensitivity enhancement in NAA by Compton suppression is also illustrated. Through a judicious combination of methodologies, practically all elements of interest in pollution and nutrition terms can be determined. (author)

Develop and validation of an analytic method for the histamine determination in fish, using chromatography liquidates of high efficiency in reverse phase with ultraviolet detection

International Nuclear Information System (INIS)

Valverde Chavarria, J. C.

1997-01-01

There were determined and optimized the reaction and conditions analysis, for the derivation of the histamine with the reagent of or-ftalaldehido (OPA), it was proven that it is possible to quantify the one derived formed at 333nm. The good conditions crhomatografics settled down for the determination of the histamine in fish by means of the analytic technique of chromatography it liquidates of high efficiency (HPLC) in reverse phase, using the derivatizacion in precolumn of the histamine with the reagent of OPA, with ultraviolet detection at 333nm. The conditions of the proposed methodology were optimized and the variables of analytic acting were validated, for the analytic quantification of the histamine in the mg g-1 environment. The applicability of the methodology was demonstrated in the histamine determination in samples of fresh fish [es

Analytical results for 544 water samples collected in the Attean Quartz Monzonite in the vicinity of Jackman, Maine

Science.gov (United States)

Ficklin, W.H.; Nowlan, G.A.; Preston, D.J.

1983-01-01

Water samples were collected in the vicinity of Jackman, Maine as a part of the study of the relationship of dissolved constituents in water to the sediments subjacent to the water. Each sample was analyzed for specific conductance, alkalinity, acidity, pH, fluoride, chloride, sulfate, phosphate, nitrate, sodium, potassium, calcium, magnesium, and silica. Trace elements determined were copper, zinc, molybdenum, lead, iron, manganese, arsenic, cobalt, nickel, and strontium. The longitude and latitude of each sample location and a sample site map are included in the report as well as a table of the analytical results.

Methodology for Validating Building Energy Analysis Simulations

Energy Technology Data Exchange (ETDEWEB)

Judkoff, R.; Wortman, D.; O' Doherty, B.; Burch, J.

2008-04-01

The objective of this report was to develop a validation methodology for building energy analysis simulations, collect high-quality, unambiguous empirical data for validation, and apply the validation methodology to the DOE-2.1, BLAST-2MRT, BLAST-3.0, DEROB-3, DEROB-4, and SUNCAT 2.4 computer programs. This report covers background information, literature survey, validation methodology, comparative studies, analytical verification, empirical validation, comparative evaluation of codes, and conclusions.

Sample preparation and EFTEM of Meat Samples for Nanoparticle Analysis in Food

International Nuclear Information System (INIS)

Lari, L; Dudkiewicz, A

2014-01-01

Nanoparticles are used in industry for personal care products and the preparation of food. In the latter application, their functions include the prevention of microbes' growth, increase of the foods nutritional value and sensory quality. EU regulations require a risk assessment of the nanoparticles used in foods and food contact materials before the products can reach the market. However, availability of validated analytical methodologies for detection and characterisation of the nanoparticles in food hampers appropriate risk assessment. As part of a research on the evaluation of the methods for screening and quantification of Ag nanoparticles in meat we have tested a new TEM sample preparation alternative to resin embedding and cryo-sectioning. Energy filtered TEM analysis was applied to evaluate thickness and the uniformity of thin meat layers acquired at increasing input of the sample demonstrating that the protocols used ensured good stability under the electron beam, reliable sample concentration and reproducibility

Sample preparation and EFTEM of Meat Samples for Nanoparticle Analysis in Food

Science.gov (United States)

Lari, L.; Dudkiewicz, A.

2014-06-01

Nanoparticles are used in industry for personal care products and the preparation of food. In the latter application, their functions include the prevention of microbes' growth, increase of the foods nutritional value and sensory quality. EU regulations require a risk assessment of the nanoparticles used in foods and food contact materials before the products can reach the market. However, availability of validated analytical methodologies for detection and characterisation of the nanoparticles in food hampers appropriate risk assessment. As part of a research on the evaluation of the methods for screening and quantification of Ag nanoparticles in meat we have tested a new TEM sample preparation alternative to resin embedding and cryo-sectioning. Energy filtered TEM analysis was applied to evaluate thickness and the uniformity of thin meat layers acquired at increasing input of the sample demonstrating that the protocols used ensured good stability under the electron beam, reliable sample concentration and reproducibility.

Analytical Chemistry Laboratory (ACL) procedure compendium

International Nuclear Information System (INIS)

1992-06-01

Covered are: analytical laboratory operations (ALO) sample receipt and control, ALO data report/package preparation review and control, single shell tank (PST) project sample tracking system, sample receiving, analytical balances, duties and responsibilities of sample custodian, sample refrigerator temperature monitoring, security, assignment of staff responsibilities, sample storage, data reporting, and general requirements for glassware

Correlated Raman micro-spectroscopy and scanning electron microscopy analyses of flame retardants in environmental samples: a micro-analytical tool for probing chemical composition, origin and spatial distribution.

Science.gov (United States)

Ghosal, Sutapa; Wagner, Jeff

2013-07-07

We present correlated application of two micro-analytical techniques: scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDS) and Raman micro-spectroscopy (RMS) for the non-invasive characterization and molecular identification of flame retardants (FRs) in environmental dusts and consumer products. The SEM/EDS-RMS technique offers correlated, morphological, molecular, spatial distribution and semi-quantitative elemental concentration information at the individual particle level with micrometer spatial resolution and minimal sample preparation. The presented methodology uses SEM/EDS analyses for rapid detection of particles containing FR specific elements as potential indicators of FR presence in a sample followed by correlated RMS analyses of the same particles for characterization of the FR sub-regions and surrounding matrices. The spatially resolved characterization enabled by this approach provides insights into the distributional heterogeneity as well as potential transfer and exposure mechanisms for FRs in the environment that is typically not available through traditional FR analysis. We have used this methodology to reveal a heterogeneous distribution of highly concentrated deca-BDE particles in environmental dust, sometimes in association with identifiable consumer materials. The observed coexistence of deca-BDE with consumer material in dust is strongly indicative of its release into the environment via weathering/abrasion of consumer products. Ingestion of such enriched FR particles in dust represents a potential for instantaneous exposure to high FR concentrations. Therefore, correlated SEM/RMS analysis offers a novel investigative tool for addressing an area of important environmental concern.

MS-Based Analytical Techniques: Advances in Spray-Based Methods and EI-LC-MS Applications

Science.gov (United States)

Medina, Isabel; Cappiello, Achille; Careri, Maria

2018-01-01

Mass spectrometry is the most powerful technique for the detection and identification of organic compounds. It can provide molecular weight information and a wealth of structural details that give a unique fingerprint for each analyte. Due to these characteristics, mass spectrometry-based analytical methods are showing an increasing interest in the scientific community, especially in food safety, environmental, and forensic investigation areas where the simultaneous detection of targeted and nontargeted compounds represents a key factor. In addition, safety risks can be identified at the early stage through online and real-time analytical methodologies. In this context, several efforts have been made to achieve analytical instrumentation able to perform real-time analysis in the native environment of samples and to generate highly informative spectra. This review article provides a survey of some instrumental innovations and their applications with particular attention to spray-based MS methods and food analysis issues. The survey will attempt to cover the state of the art from 2012 up to 2017.

Determination of 7BE in soil sample by gamma spectrometry for erosion researchs

International Nuclear Information System (INIS)

Esquivel, Alexander D.; Kastner, Geraldo F.; Amaral, Angela M.; Monteiro, Roberto Pellacani G.; Moreira, Rubens M.

2015-01-01

Cosmogenic 7 Be is a natural radiotracer produced in the stratosphere and troposphere and reached to the Earth surface via wet and dry fallout and hence its measurement for research of erosion in soils is very significant. The 7 Be radio analyse based on gamma spectrometry technique has been a routine methodology for decades and although is the reference procedure is not free of analytical interference. 7 Be is a β-γ emitting radionuclide (Eγ = 477.59 keV, T½ = 53.12d) and depending on the chemical profile of the soil its determination is susceptible to 228 Ac (E γ = 478.40 keV, T½ = 6.15h) interference. The aim of this work was to establish an analytical protocol for the 7 Be determination in soil samples from Juatuba-Mg region in different sampling periods of dry and rainy seasons for erosion studies and to establish some methodologies for evaluating and correcting the interference level of 228 Ac in the 7 Be activity measurements by gamma spectrometry. (author)

Co marker determination in rumen liquid sample by energy dispersive X-ray fluorescence

Energy Technology Data Exchange (ETDEWEB)

Almeida, Eduardo de; Nascimento Filho, Virgilio F.; Massoni, Paulo R. [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil). Lab. de Instrumentacao Nuclear (LIN)]. E-mail: edualm@usp.br; Leite, Laudi C.; Lanna, Dante P.D. [Escola Superior de Agricultura ' Luiz de Queiroz' (ESALQ/USP), Piracicaba, SP (Brazil). Dept. de Zootecnia. Lab. de Anatomia e Fisiologia Animal (LAFA)]. E-mail: lcleite@ciagri.usp.br

2007-07-01

The Co element is used in nutritional studies as marker. This paper describes an analytical methodology for Co determination in rumen liquid sample using energy dispersive X-ray spectrometry (EDXRF). 200 {mu}L of the sample were dried at 60 deg C on 6.35 {mu}m Mylar film. Ga was used as internal standard. The excitation was carried out utilizing Mo target X-ray tube (Zr filter) at 30 kV / 20 mA. The acquisition time was 200 s. The accuracy of this methodology was assessed through standard addition method, the recovery obtained was 98.7 % for Co. The detection limit was 0.15 mg / L for this element. (author)

Co marker determination in rumen liquid sample by energy dispersive X-ray fluorescence

International Nuclear Information System (INIS)

Almeida, Eduardo de; Nascimento Filho, Virgilio F.; Massoni, Paulo R.; Leite, Laudi C.; Lanna, Dante P.D.

2007-01-01

The Co element is used in nutritional studies as marker. This paper describes an analytical methodology for Co determination in rumen liquid sample using energy dispersive X-ray spectrometry (EDXRF). 200 μL of the sample were dried at 60 deg C on 6.35 μm Mylar film. Ga was used as internal standard. The excitation was carried out utilizing Mo target X-ray tube (Zr filter) at 30 kV / 20 mA. The acquisition time was 200 s. The accuracy of this methodology was assessed through standard addition method, the recovery obtained was 98.7 % for Co. The detection limit was 0.15 mg / L for this element. (author)

Determination of insoluble soap in agricultural soil and sewage sludge samples by liquid chromatography with ultraviolet detection.

Science.gov (United States)

Cantarero, Samuel; Zafra-Gómez, Alberto; Ballesteros, Oscar; Navalón, Alberto; Vílchez, José L; Crovetto, Guillermo; Verge, Coral; de Ferrer, Juan A

2010-11-01

We have developed a new analytical procedure for determining insoluble Ca and Mg fatty acid salts (soaps) in agricultural soil and sewage sludge samples. The number of analytical methodologies that focus in the determination of insoluble soap salts in different environmental compartments is very limited. In this work, we propose a methodology that involves a sample clean-up step with petroleum ether to remove soluble salts and a conversion of Ca and Mg insoluble salts into soluble potassium salts using tripotassium ethylenediaminetetraacetate salt and potassium carbonate, followed by the extraction of analytes from the samples using microwave-assisted extraction with methanol. An improved esterification procedure using 2,4-dibromoacetophenone before the liquid chromatography with ultraviolet detection analysis also has been developed. The absence of matrix effect was demonstrated with two fatty acid Ca salts that are not commercial and are never detected in natural samples (C₁₃:₀ and C₁₇:₀). Therefore, it was possible to evaluate the matrix effect because both standards have similar environmental behavior (adsorption and precipitation) to commercial soaps (C₁₀:₀) to C₁₈:₀). We also studied the effect of the different variables on the clean-up, the conversion of Ca soap, and the extraction and derivatization procedures. The quantification limits found ranged from 0.4 to 0.8 mg/kg. The proposed method was satisfactorily applied for the development of a study on soap behavior in agricultural soil and sewage sludge samples. © 2010 SETAC.

Methodology Series Module 5: Sampling Strategies.

Science.gov (United States)

Setia, Maninder Singh

2016-01-01

Once the research question and the research design have been finalised, it is important to select the appropriate sample for the study. The method by which the researcher selects the sample is the ' Sampling Method'. There are essentially two types of sampling methods: 1) probability sampling - based on chance events (such as random numbers, flipping a coin etc.); and 2) non-probability sampling - based on researcher's choice, population that accessible & available. Some of the non-probability sampling methods are: purposive sampling, convenience sampling, or quota sampling. Random sampling method (such as simple random sample or stratified random sample) is a form of probability sampling. It is important to understand the different sampling methods used in clinical studies and mention this method clearly in the manuscript. The researcher should not misrepresent the sampling method in the manuscript (such as using the term ' random sample' when the researcher has used convenience sample). The sampling method will depend on the research question. For instance, the researcher may want to understand an issue in greater detail for one particular population rather than worry about the ' generalizability' of these results. In such a scenario, the researcher may want to use ' purposive sampling' for the study.

Methodology series module 5: Sampling strategies

Directory of Open Access Journals (Sweden)

Maninder Singh Setia

2016-01-01

Full Text Available Once the research question and the research design have been finalised, it is important to select the appropriate sample for the study. The method by which the researcher selects the sample is the 'Sampling Method'. There are essentially two types of sampling methods: 1 probability sampling – based on chance events (such as random numbers, flipping a coin etc.; and 2 non-probability sampling – based on researcher's choice, population that accessible & available. Some of the non-probability sampling methods are: purposive sampling, convenience sampling, or quota sampling. Random sampling method (such as simple random sample or stratified random sample is a form of probability sampling. It is important to understand the different sampling methods used in clinical studies and mention this method clearly in the manuscript. The researcher should not misrepresent the sampling method in the manuscript (such as using the term 'random sample' when the researcher has used convenience sample. The sampling method will depend on the research question. For instance, the researcher may want to understand an issue in greater detail for one particular population rather than worry about the 'generalizability' of these results. In such a scenario, the researcher may want to use 'purposive sampling' for the study.

Neutron activation analysis technique and X-ray fluorescence in bovine liver sample

International Nuclear Information System (INIS)

Maihara, V.A.; Favaro, D.I.T.; Vasconcellos, M.B.A.; Sato, I.M.; Salvador, V.L.

2002-01-01

Many analytical techniques have been used in food and diet analysis in order to determine a great number of nutritional elements, ranging from percentage to ng g -1 , with high sensitivity and accuracy. Instrumental Neutron activation Analysis (INAA) has been employed to certificate many trace elements in biological reference materials. More recently, the X-Ray Fluorescence (FRX-WD) has been also used to determine some essential elements in food samples. The INAA has been applied in nutrition studies in our laboratory at IPEN since the 80 s. For the development of analytical methodologies the use of the reference materials with the same characteristics of the sample analyzed is essential. Several Brazilian laboratories do not have conditions to use these materials due their high cost.In this paper preliminary results of commercial bovine liver sample analyses obtained by INAA and WD-XRF methods are presented. This sample was prepared to be a Brazilian candidate of reference material for a group of laboratories participating in a research project sponsored by FAPESP. The concentrations of some elements like Cl, K, Na, P, S and trace elements Br, Ca, Co, Cu, Fe, Mg, Mn, Mo, Rb, Se and Zn were determined by INAA and WD-XFR. For validation methodology of both techniques, NIST SRM 1577b Bovine Liver reference material was analyzed and the detection limits were calculated. The concentrations of elements determined by both analytical techniques were compared by using the Student's t-test and for Cl, Cu, Fe, K, Mg, Na, Rn and Zn the results do show no statistical difference for 95% significance level. (author)

Liquid phase micro-extraction: Towards the green methodology for ultratrace metals determination in aquatic ecosystems

Directory of Open Access Journals (Sweden)

López-López J. A.

2013-04-01

Full Text Available Heavy metals are normally found, in natural waters, in very low concentrations. Some of them are essential for life in low level; however, in higher level they are toxic. Therefore, analyzing their bio-available fraction is of main interest. Standard methodology is based in the collection of a number of samples from a water body. Collected samples must be stored, pre-treated and then analyzed. Pre-treatment usually involves pre-concentrating the metal, with the corresponding risk of contamination or loss of analyte. This way, punctual information is obtained from every sampling campaign. As an alternative, passive sampling techniques allow the continuous and coupled sampling-pre-treatment for heavy metals analysis, giving a better approach in the characterization of the studied water body. Liquid phase micro-extraction (LPME is a green analytical alternative for liquid-liquid extraction that promotes a reduction of sample volume, solvent needed and waste generation. Using these systems, polypropylene hollow fibers (HF with pores in their walls can be used. A few micro-liters of organic solvent are supported in the pores. The sample is placed in the outer part of the fiber and a receiving phase is placed in its inner part, allowing continuous liquid extraction of the metal from the sample. Several fibers with different physical features have been employed to analyzed total concentration and bio-availability of some heavy metals (Ag, Ni, Cu in natural water samples. Thanks to fibers configuration, devices for passive sampling based in HF-LPME could be designed. Advantages of this methodology over existing ones are supported because the receiving phase is liquid. As a consequence, retained metals do not need to be eluted from the acceptor prior to instrumental analysis.

Automated Ground-Water Sampling and Analysis of Hexavalent Chromium using a “Universal” Sampling/Analytical System

Directory of Open Access Journals (Sweden)

Richard J. Venedam

2005-02-01

Full Text Available The capabilities of a “universal platform” for the deployment of analyticalsensors in the field for long-term monitoring of environmental contaminants were expandedin this investigation. The platform was previously used to monitor trichloroethene inmonitoring wells and at groundwater treatment systems (1,2. The platform was interfacedwith chromium (VI and conductivity analytical systems to monitor shallow wells installedadjacent to the Columbia River at the 100-D Area of the Hanford Site, Washington. Agroundwater plume of hexavalent chromium is discharging into the Columbia River throughthe gravels beds used by spawning salmon. The sampling/analytical platform was deployedfor the purpose of collecting data on subsurface hexavalent chromium concentrations atmore frequent intervals than was possible with the previous sampling and analysis methodsemployed a the Site.

Quantile arithmetic methodology for uncertainty propagation in fault trees

International Nuclear Information System (INIS)

Abdelhai, M.; Ragheb, M.

1986-01-01

A methodology based on quantile arithmetic, the probabilistic analog to interval analysis, is proposed for the computation of uncertainties propagation in fault tree analysis. The basic events' continuous probability density functions (pdf's) are represented by equivalent discrete distributions by dividing them into a number of quantiles N. Quantile arithmetic is then used to performthe binary arithmetical operations corresponding to the logical gates in the Boolean expression of the top event expression of a given fault tree. The computational advantage of the present methodology as compared with the widely used Monte Carlo method was demonstrated for the cases of summation of M normal variables through the efficiency ratio defined as the product of the labor and error ratios. The efficiency ratio values obtained by the suggested methodology for M = 2 were 2279 for N = 5, 445 for N = 25, and 66 for N = 45 when compared with the results for 19,200 Monte Carlo samples at the 40th percentile point. Another advantage of the approach is that the exact analytical value of the median is always obtained for the top event

SEMANTIC NETWORKS: THEORETICAL, TECHNICAL, METHODOLOGIC AND ANALYTICAL ASPECTS

Directory of Open Access Journals (Sweden)

José Ángel Vera Noriega

2005-09-01

Full Text Available This work is a review of the methodological procedures and cares for the measurement of the connotative meanings which will be used in the elaboration of instruments with ethnic validity. Beginning from the techniques originally proposed by Figueroa et al. (1981 and later described by Lagunes (1993, the intention is to offer a didactic panorama to carry out the measurement by semantic networks introducing some recommendations derived from the studies performed with this method.

Methodological integrative review of the work sampling technique used in nursing workload research.

Science.gov (United States)

Blay, Nicole; Duffield, Christine M; Gallagher, Robyn; Roche, Michael

2014-11-01

To critically review the work sampling technique used in nursing workload research. Work sampling is a technique frequently used by researchers and managers to explore and measure nursing activities. However, work sampling methods used are diverse making comparisons of results between studies difficult. Methodological integrative review. Four electronic databases were systematically searched for peer-reviewed articles published between 2002-2012. Manual scanning of reference lists and Rich Site Summary feeds from contemporary nursing journals were other sources of data. Articles published in the English language between 2002-2012 reporting on research which used work sampling to examine nursing workload. Eighteen articles were reviewed. The review identified that the work sampling technique lacks a standardized approach, which may have an impact on the sharing or comparison of results. Specific areas needing a shared understanding included the training of observers and subjects who self-report, standardization of the techniques used to assess observer inter-rater reliability, sampling methods and reporting of outcomes. Work sampling is a technique that can be used to explore the many facets of nursing work. Standardized reporting measures would enable greater comparison between studies and contribute to knowledge more effectively. Author suggestions for the reporting of results may act as guidelines for researchers considering work sampling as a research method. © 2014 John Wiley & Sons Ltd.

Radio drama adaptations: an approach towards an analytical methodology

NARCIS (Netherlands)

Huwiler, E.

2010-01-01

This article establishes a methodology with which radio drama pieces can be analysed. It thereby integrates all features the art form has to offer: voices, music, noises, but also technical features like cutting and mixing contribute to the narrative that is being told. This approach emphasizes the

The SRS analytical laboratories strategic plan

International Nuclear Information System (INIS)

Hiland, D.E.

1993-01-01

There is an acute shortage of Savannah River Site (SRS) analytical laboratory capacity to support key Department of Energy (DOE) environmental restoration and waste management (EM) programs while making the transition from traditional defense program (DP) missions as a result of the cessation of the Cold War. This motivated Westinghouse Savannah River Company (WSRC) to develop an open-quotes Analytical Laboratories Strategic Planclose quotes (ALSP) in order to provide appropriate input to SRS operating plans and justification for proposed analytical laboratory projects. The methodology used to develop this plan is applicable to all types of strategic planning

Immediate drop on demand technology (I-DOT) coupled with mass spectrometry via an open port sampling interface.

Science.gov (United States)

Van Berkel, Gary J; Kertesz, Vilmos; Boeltz, Harry

2017-11-01

The aim of this work was to demonstrate and evaluate the analytical performance of coupling the immediate drop on demand technology to a mass spectrometer via the recently introduced open port sampling interface and ESI. Methodology & results: A maximum sample analysis throughput of 5 s per sample was demonstrated. Signal reproducibility was 10% or better as demonstrated by the quantitative analysis of propranolol and its stable isotope-labeled internal standard propranolol-d7. The ability of the system to multiply charge and analyze macromolecules was demonstrated using the protein cytochrome c. This immediate drop on demand technology/open port sampling interface/ESI-MS combination allowed for the quantitative analysis of relatively small mass analytes and was used for the identification of macromolecules like proteins.

Methodology Series Module 5: Sampling Strategies

Science.gov (United States)

Setia, Maninder Singh

2016-01-01

Once the research question and the research design have been finalised, it is important to select the appropriate sample for the study. The method by which the researcher selects the sample is the ‘ Sampling Method’. There are essentially two types of sampling methods: 1) probability sampling – based on chance events (such as random numbers, flipping a coin etc.); and 2) non-probability sampling – based on researcher's choice, population that accessible & available. Some of the non-probability sampling methods are: purposive sampling, convenience sampling, or quota sampling. Random sampling method (such as simple random sample or stratified random sample) is a form of probability sampling. It is important to understand the different sampling methods used in clinical studies and mention this method clearly in the manuscript. The researcher should not misrepresent the sampling method in the manuscript (such as using the term ‘ random sample’ when the researcher has used convenience sample). The sampling method will depend on the research question. For instance, the researcher may want to understand an issue in greater detail for one particular population rather than worry about the ‘ generalizability’ of these results. In such a scenario, the researcher may want to use ‘ purposive sampling’ for the study. PMID:27688438

Possibilities for decreasing detection limits of analytical methods for determination of transformation products of unsymmetrical dimethylhydrazine in environmental samples

Directory of Open Access Journals (Sweden)

Bulat Kenessov

2015-12-01

Full Text Available Most rockets of middle and heavy class launched from Kazakhstan, Russia, China and other countries still use highly toxic unsymmetrical dimethylhydrazine (UDMH as a liquid propellant. Study of migration, distribution and accumulation of UDMH transformation products in environment and human health impact assessment of space rocket activity are currently complicated due to the absence of analytical methods allowing detection of trace concentrations of these compounds in analyzed samples. This paper reviews methods and approaches, which can be applied for development of such methods. Detection limits at a part-per-trillion (ppt level may be achieved using most selective and sensitive methods based on gas or liquid chromatography in combination of tandem or high-resolution mass spectrometry. In addition, 1000-fold concentration of samples or integrated sample preparation methods, e.g., dynamic headspace extraction, are required. Special attention during development and application of such methods must be paid to purity of laboratory air, reagents, glassware and analytical instruments.

THE CREATION OF ANALYTICAL PREDICATION CONCEPT IN MULTILEVEL ORGANIZATION SYSTEM MANAGEMENT

Directory of Open Access Journals (Sweden)

O. M. Pisareva

2013-01-01

Full Text Available This article deals with analytical and forecasting methodology problems in the integrated business systems management. The theoretical framework of analytical predication concept in multilevel organization systems is presented.

Use of reference materials for validating analytical methods. Applied to the determination of As, Co, Na, Hg, Se and Fe using neutron activation analysis

International Nuclear Information System (INIS)

Munoz, L; Andonie, O; Kohnenkamp, I

2000-01-01

The main purpose of an analytical laboratory is to provide reliable information on the nature and composition of the materials submitted for analysis. This purpose can only be attained if analytical methodologies that have the attributes of accuracy, precision, specificity and sensitivity, among others, are used. The process by which these attributes are evaluated is called validation of the analytical method. The Chilean Nuclear Energy Commission's Neutron Activation Analysis Laboratory is applying a quality guarantee program to ensure the quality of its analytical results, which aims, as well, to attain accreditation for some of its measurements. Validation of the analytical methodologies used is an essential part of applying this program. There are many forms of validation, from comparison with reference techniques to participation in inter-comparison rounds. Certified reference materials were used in this work in order to validate the application of neutron activation analysis in determining As, Co, Na, Hg, Se and Fe in shellfish samples. The use of reference materials was chosen because it is a simple option that easily detects sources of systematic errors. Neutron activation analysis is an instrumental analytical method that does not need chemical treatment and that is based on processes which take place in the nuclei of atoms, making the matrix effects unimportant and different biological reference materials can be used. The following certified reference materials were used for validating the method used: BCR human hair 397, NRCC dogfish muscle DORM-2, NRCC -dogfish liver DOLT-2, NIST - oyster tissue 1566, NIES - mussel 6 and BCR - tuna fish 464. The reference materials were analyzed using the procedure developed for the shellfish samples and the above-mentioned elements were determined. With the results obtained, the parameters of accuracy, precision, detection limit, quantification limit and uncertainty associated with the method were determined for each

Development of analytical techniques for water and environmental samples (2)

Energy Technology Data Exchange (ETDEWEB)

Eum, Chul Hun; Jeon, Chi Wan; Jung, Kang Sup; Song, Kyung Sun; Kim, Sang Yeon [Korea Institute of Geology Mining and Materials, Taejon (Korea)

1998-12-01

The purpose of this study is to develop new analytical methods with good detection limit for toxic inorganic and organic compounds. The analyses of CN, organic acids, particulate materials in environmental samples have been done using several methods such as Ion Chromatography, SPE, SPME, GC/MS, GC/FID, SPLITT (split-flow thin cell fractionation) during the second year of this project. Advantage and disadvantage of several distillation method (by KS, JIS, EPA) for CN analysis in wastewater were investigated. As the results, we proposed new distillation apparatus for CN analysis, which was proved to be simpler, faster and to get better recovery than conventional apparatus. And ion chromatograph/pulsed amperometric detector (IC/PAD) system instead of colorimetry for CN detection was setup to solve matrix interference. And SPE(solid phase extraction) and SPME (solid phase micro extraction) as liquid-solid extraction technique were applied to the analysis of phenols in wastewater. Optimum experimental conditions and factors influencing analytical results were determined. From these results, It could be concluded that C{sub 18} cartridge and polystyrene-divinylbenzene disk in SPE method, polyacrylate fiber in SPME were proper solid phase adsorbent for phenol. Optimum conditions to analyze phenol derivatives simultaneously were established. Also, Continuous SPLITT (Split-flow thin cell) Fractionation (CSF) is a new preparative separation technique that is useful for fractionation of particulate and macromolecular materials. CSF is carried out in a thin ribbon-like channel equipped with two splitters at both inlet and outlet of the channel. In this work, we set up a new CSF system, and tested using polystyrene latex standard particles. And then we fractionated particles contained in air and underground water based on their sedimentation coefficients using CSF. (author). 27 refs., 13 tabs., 31 figs.

Effects of fecal sampling on preanalytical and analytical phases in quantitative fecal immunochemical tests for hemoglobin.

Science.gov (United States)

Rapi, Stefano; Berardi, Margherita; Cellai, Filippo; Ciattini, Samuele; Chelazzi, Laura; Ognibene, Agostino; Rubeca, Tiziana

2017-07-24

Information on preanalytical variability is mandatory to bring laboratories up to ISO 15189 requirements. Fecal sampling is greatly affected by lack of harmonization in laboratory medicine. The aims of this study were to obtain information on the devices used for fecal sampling and to explore the effect of different amounts of feces on the results from the fecal immunochemical test for hemoglobin (FIT-Hb). Four commercial sample collection devices for quantitative FIT-Hb measurements were investigated. The volume of interest (VOI) of the probes was measured from diameter and geometry. Quantitative measurements of the mass of feces were carried out by gravimetry. The effects of an increased amount of feces on the analytical environment were investigated measuring the Hb values with a single analytical method. VOI was 8.22, 7.1 and 9.44 mm3 for probes that collected a target of 10 mg of feces, and 3.08 mm3 for one probe that targeted 2 mg of feces. The ratio between recovered and target amounts of devices ranged from 56% to 121%. Different changes in the measured Hb values were observed, in adding increasing amounts of feces in commercial buffers. The amounts of collected materials are related to the design of probes. Three out 4 manufacturers declare the same target amount using different sampling volumes and obtaining different amounts of collected materials. The introduction of a standard probes to reduce preanalytical variability could be an useful step for fecal test harmonization and to fulfill the ISO 15189 requirements.

Municipal solid waste composition: Sampling methodology, statistical analyses, and case study evaluation

International Nuclear Information System (INIS)

Edjabou, Maklawe Essonanawe; Jensen, Morten Bang; Götze, Ramona; Pivnenko, Kostyantyn; Petersen, Claus; Scheutz, Charlotte; Astrup, Thomas Fruergaard

2015-01-01

Highlights: • Tiered approach to waste sorting ensures flexibility and facilitates comparison of solid waste composition data. • Food and miscellaneous wastes are the main fractions contributing to the residual household waste. • Separation of food packaging from food leftovers during sorting is not critical for determination of the solid waste composition. - Abstract: Sound waste management and optimisation of resource recovery require reliable data on solid waste generation and composition. In the absence of standardised and commonly accepted waste characterisation methodologies, various approaches have been reported in literature. This limits both comparability and applicability of the results. In this study, a waste sampling and sorting methodology for efficient and statistically robust characterisation of solid waste was introduced. The methodology was applied to residual waste collected from 1442 households distributed among 10 individual sub-areas in three Danish municipalities (both single and multi-family house areas). In total 17 tonnes of waste were sorted into 10–50 waste fractions, organised according to a three-level (tiered approach) facilitating comparison of the waste data between individual sub-areas with different fractionation (waste from one municipality was sorted at “Level III”, e.g. detailed, while the two others were sorted only at “Level I”). The results showed that residual household waste mainly contained food waste (42 ± 5%, mass per wet basis) and miscellaneous combustibles (18 ± 3%, mass per wet basis). The residual household waste generation rate in the study areas was 3–4 kg per person per week. Statistical analyses revealed that the waste composition was independent of variations in the waste generation rate. Both, waste composition and waste generation rates were statistically similar for each of the three municipalities. While the waste generation rates were similar for each of the two housing types (single

Municipal solid waste composition: Sampling methodology, statistical analyses, and case study evaluation

Energy Technology Data Exchange (ETDEWEB)

Edjabou, Maklawe Essonanawe, E-mail: vine@env.dtu.dk [Department of Environmental Engineering, Technical University of Denmark, 2800 Kgs. Lyngby (Denmark); Jensen, Morten Bang; Götze, Ramona; Pivnenko, Kostyantyn [Department of Environmental Engineering, Technical University of Denmark, 2800 Kgs. Lyngby (Denmark); Petersen, Claus [Econet AS, Omøgade 8, 2.sal, 2100 Copenhagen (Denmark); Scheutz, Charlotte; Astrup, Thomas Fruergaard [Department of Environmental Engineering, Technical University of Denmark, 2800 Kgs. Lyngby (Denmark)

2015-02-15

Highlights: • Tiered approach to waste sorting ensures flexibility and facilitates comparison of solid waste composition data. • Food and miscellaneous wastes are the main fractions contributing to the residual household waste. • Separation of food packaging from food leftovers during sorting is not critical for determination of the solid waste composition. - Abstract: Sound waste management and optimisation of resource recovery require reliable data on solid waste generation and composition. In the absence of standardised and commonly accepted waste characterisation methodologies, various approaches have been reported in literature. This limits both comparability and applicability of the results. In this study, a waste sampling and sorting methodology for efficient and statistically robust characterisation of solid waste was introduced. The methodology was applied to residual waste collected from 1442 households distributed among 10 individual sub-areas in three Danish municipalities (both single and multi-family house areas). In total 17 tonnes of waste were sorted into 10–50 waste fractions, organised according to a three-level (tiered approach) facilitating comparison of the waste data between individual sub-areas with different fractionation (waste from one municipality was sorted at “Level III”, e.g. detailed, while the two others were sorted only at “Level I”). The results showed that residual household waste mainly contained food waste (42 ± 5%, mass per wet basis) and miscellaneous combustibles (18 ± 3%, mass per wet basis). The residual household waste generation rate in the study areas was 3–4 kg per person per week. Statistical analyses revealed that the waste composition was independent of variations in the waste generation rate. Both, waste composition and waste generation rates were statistically similar for each of the three municipalities. While the waste generation rates were similar for each of the two housing types (single

Maybe Small Is Too Small a Term: Introduction to Advancing Small Sample Prevention Science.

Science.gov (United States)

Fok, Carlotta Ching Ting; Henry, David; Allen, James

2015-10-01

Prevention research addressing health disparities often involves work with small population groups experiencing such disparities. The goals of this special section are to (1) address the question of what constitutes a small sample; (2) identify some of the key research design and analytic issues that arise in prevention research with small samples; (3) develop applied, problem-oriented, and methodologically innovative solutions to these design and analytic issues; and (4) evaluate the potential role of these innovative solutions in describing phenomena, testing theory, and evaluating interventions in prevention research. Through these efforts, we hope to promote broader application of these methodological innovations. We also seek whenever possible, to explore their implications in more general problems that appear in research with small samples but concern all areas of prevention research. This special section includes two sections. The first section aims to provide input for researchers at the design phase, while the second focuses on analysis. Each article describes an innovative solution to one or more challenges posed by the analysis of small samples, with special emphasis on testing for intervention effects in prevention research. A concluding article summarizes some of their broader implications, along with conclusions regarding future directions in research with small samples in prevention science. Finally, a commentary provides the perspective of the federal agencies that sponsored the conference that gave rise to this special section.

Analytical Solution of General Bagley-Torvik Equation

OpenAIRE

William Labecca; Osvaldo Guimarães; José Roberto C. Piqueira

2015-01-01

Bagley-Torvik equation appears in viscoelasticity problems where fractional derivatives seem to play an important role concerning empirical data. There are several works treating this equation by using numerical methods and analytic formulations. However, the analytical solutions presented in the literature consider particular cases of boundary and initial conditions, with inhomogeneous term often expressed in polynomial form. Here, by using Laplace transform methodology, the general inhomoge...

Ultratrace analysis of polychlorinated biphenyls (PCBs) and their hydroxylated metabolites (OH-PCBs) in human serum and cerebrospinal fluid (CSF) samples

Energy Technology Data Exchange (ETDEWEB)

Takasuga, T.; Senthilkumar, K.; Watanabe, K.; Takemori, H. [Shimadzu Techno Research, Inc., Kyoto (Japan); Shoda, T. [Ehime Univ. Medical Research Center, Matsuyama (Japan); Kuroda, Y. [Tokyo Metropolitan Inst. for Neuroscience, Tokyo (Japan)

2004-09-15

In the present study, we established pretreatment and high sensitivity analytical method of polychlorinated biphenyls (PCBs) and their hydroxylated metabolites (OH-PCBs) in serum and cerebrospinal fluid (CSF) of humans for the first time. Analyzing serum and CSF samples from humans found unique because PCBs behavior and metabolism could be discerned. Furthermore, so far studies reported concentrations of OH-PCBs in wildlife samples obtained by HRGC-LRMS or GC-ECD data. In this study, we established cleanup and analytical methods by high resolution gas chromatography-high resolution mass spectrometry (HRGC-HRMS) using 1 mL of sample. Mainly, total PCBs and OH-PCBs in the CSF were extracted by specialized developed method. Using this method, PCBs and OH-PCBs could be determined swiftly. Based on this method, major OH-PCB congeners were detected from human, serum, CSF, control serum and Rhesus monkey plasma. Present methodology developed based on the isotope dilution technique using OH-PCBs standard and thus we suggest the present methodology could apply for ultra trace analysis of OHPCBs as well as total PCBs in human samples.

Sequential automated fusion/extraction chromatography methodology for the dissolution of uranium in environmental samples for mass spectrometric determination

Energy Technology Data Exchange (ETDEWEB)

Milliard, Alex; Durand-Jezequel, Myriam [Laboratoire de Radioecologie, Departement de chimie, Universite Laval, 1045 Avenue de la Medecine, Quebec, QC, G1V 0A6 (Canada); Lariviere, Dominic, E-mail: dominic.lariviere@chm.ulaval.ca [Laboratoire de Radioecologie, Departement de chimie, Universite Laval, 1045 Avenue de la Medecine, Quebec, QC, G1V 0A6 (Canada)

2011-01-17

An improved methodology has been developed, based on dissolution by automated fusion followed by extraction chromatography for the detection and quantification of uranium in environmental matrices by mass spectrometry. A rapid fusion protocol (<8 min) was investigated for the complete dissolution of various samples. It could be preceded, if required, by an effective ashing procedure using the M4 fluxer and a newly designed platinum lid. Complete dissolution of the sample was observed and measured using standard reference materials (SRMs) and experimental data show no evidence of cross-contamination of crucibles when LiBO{sub 2}/LiBr melts were used. The use of a M4 fusion unit also improved repeatability in sample preparation over muffle furnace fusion. Instrumental issues originating from the presence of high salt concentrations in the digestate after lithium metaborate fusion was also mitigated using an extraction chromatography (EXC) protocol aimed at removing lithium and interfering matrix constituants prior to the elution of uranium. The sequential methodology, which can be performed simultaneously on three samples, requires less than 20 min per sample for fusion and separation. It was successfully coupled to inductively coupled plasma mass spectrometry (ICP-MS) achieving detection limits below 100 pg kg{sup -1} for 5-300 mg of sample.

SPIDIA-DNA: An External Quality Assessment for the pre-analytical phase of blood samples used for DNA-based analyses

Czech Academy of Sciences Publication Activity Database

Malentacchi, F.; Pazzagli, M.; Simi, L.; Orlando, C.; Wyrich, R.; Hartmann, C.C.; Verderio, P.; Pizzamiglio, S.; Ciniselli, C.M.; Tichopád, Aleš; Kubista, Mikael; Gelmini, S.

-, č. 424 (2013), s. 274-286 ISSN 0009-8981 Institutional research plan: CEZ:AV0Z50520701 Keywords : Pre-analytical phase * DNA quality * Blood samples Subject RIV: EB - Genetics ; Molecular Biology Impact factor: 2.764, year: 2013

[Patient identification errors and biological samples in the analytical process: Is it possible to improve patient safety?].

Science.gov (United States)

Cuadrado-Cenzual, M A; García Briñón, M; de Gracia Hills, Y; González Estecha, M; Collado Yurrita, L; de Pedro Moro, J A; Fernández Pérez, C; Arroyo Fernández, M

2015-01-01

Patient identification errors and biological samples are one of the problems with the highest risk factor in causing an adverse event in the patient. To detect and analyse the causes of patient identification errors in analytical requests (PIEAR) from emergency departments, and to develop improvement strategies. A process and protocol was designed, to be followed by all professionals involved in the requesting and performing of laboratory tests. Evaluation and monitoring indicators of PIEAR were determined, before and after the implementation of these improvement measures (years 2010-2014). A total of 316 PIEAR were detected in a total of 483,254 emergency service requests during the study period, representing a mean of 6.80/10,000 requests. Patient identification failure was the most frequent in all the 6-monthly periods assessed, with a significant difference (Perrors. However, we must continue working with this strategy, promoting a culture of safety for all the professionals involved, and trying to achieve the goal that 100% of the analytical and samples are properly identified. Copyright © 2015 SECA. Published by Elsevier Espana. All rights reserved.

Big data analytics in healthcare: promise and potential.

Science.gov (United States)

Raghupathi, Wullianallur; Raghupathi, Viju

2014-01-01

To describe the promise and potential of big data analytics in healthcare. The paper describes the nascent field of big data analytics in healthcare, discusses the benefits, outlines an architectural framework and methodology, describes examples reported in the literature, briefly discusses the challenges, and offers conclusions. The paper provides a broad overview of big data analytics for healthcare researchers and practitioners. Big data analytics in healthcare is evolving into a promising field for providing insight from very large data sets and improving outcomes while reducing costs. Its potential is great; however there remain challenges to overcome.

Methodology Series Module 5: Sampling Strategies

OpenAIRE

Setia, Maninder Singh

2016-01-01

Once the research question and the research design have been finalised, it is important to select the appropriate sample for the study. The method by which the researcher selects the sample is the ? Sampling Method?. There are essentially two types of sampling methods: 1) probability sampling ? based on chance events (such as random numbers, flipping a coin etc.); and 2) non-probability sampling ? based on researcher's choice, population that accessible & available. Some of the non-probabilit...

Use of NIR spectroscopy and multivariate process spectra calibration methodology for pharmaceutical solid samples analysis

OpenAIRE

Cárdenas Espitia, Vanessa

2012-01-01

Accomplish high quality of final products in pharmaceutical industry is a challenge that requires the control and supervision of all the manufacturing steps. This request created the necessity of developing fast and accurate analytical methods. Near infrared spectroscopy together with chemometrics, fulfill this growing demand. The high speed providing relevant information and the versatility of its application to different types of samples lead these combined techniques as one of the most app...

Dry sample storage system for an analytical laboratory supporting plutonium processing

International Nuclear Information System (INIS)

Treibs, H.A.; Hartenstein, S.D.; Griebenow, B.L.; Wade, M.A.

1990-01-01

The Special Isotope Separation (SIS) plant is designed to provide removal of undesirable isotopes in fuel grade plutonium by the atomic vapor laser isotope separation (AVLIS) process. The AVLIS process involves evaporation of plutonium metal, and passage of an intense beam of light from a laser through the plutonium vapor. The laser beam consists of several discrete wavelengths, tuned to the precise wavelength required to ionize the undesired isotopes. These ions are attracted to charged plates, leaving the bulk of the plutonium vapor enriched in the desired isotopes to be collected on a cold plate. Major portions of the process consist of pyrochemical processes, including direct reduction of the plutonium oxide feed material with calcium metal, and aqueous processes for purification of plutonium in residues. The analytical laboratory for the plant is called the Material and Process Control Laboratory (MPCL), and provides for the analysis of solid and liquid process samples

Development of analytical methods for the separation of plutonium, americium, curium and neptunium from environmental samples

Energy Technology Data Exchange (ETDEWEB)

Salminen, S.

2009-07-01

In this work, separation methods have been developed for the analysis of anthropogenic transuranium elements plutonium, americium, curium and neptunium from environmental samples contaminated by global nuclear weapons testing and the Chernobyl accident. The analytical methods utilized in this study are based on extraction chromatography. Highly varying atmospheric plutonium isotope concentrations and activity ratios were found at both Kurchatov (Kazakhstan), near the former Semipalatinsk test site, and Sodankylae (Finland). The origin of plutonium is almost impossible to identify at Kurchatov, since hundreds of nuclear tests were performed at the Semipalatinsk test site. In Sodankylae, plutonium in the surface air originated from nuclear weapons testing, conducted mostly by USSR and USA before the sampling year 1963. The variation in americium, curium and neptunium concentrations was great as well in peat samples collected in southern and central Finland in 1986 immediately after the Chernobyl accident. The main source of transuranium contamination in peats was from global nuclear test fallout, although there are wide regional differences in the fraction of Chernobyl-originated activity (of the total activity) for americium, curium and neptunium. The separation methods developed in this study yielded good chemical recovery for the elements investigated and adequately pure fractions for radiometric activity determination. The extraction chromatographic methods were faster compared to older methods based on ion exchange chromatography. In addition, extraction chromatography is a more environmentally friendly separation method than ion exchange, because less acidic waste solutions are produced during the analytical procedures. (orig.)

Analytical Issues on the Determination of Carotenoids in Microalgae by Liquid Chromatography with Diode Array Detector; Aspectos Analiticos sobre la Determinacion de Compuestos Carotenoides en Microalgas mediante Cromatografia de Liquidos con Detector de Diodos

Energy Technology Data Exchange (ETDEWEB)

Garcia, S.; Perez, R. M.

2012-04-11

A preliminary study of literature review on the determination of carotenoids in microalgae samples by HPLC with diode array detector is presented. Main objective has been focused to compile data from literature and based on the main aspects of the analytical methodology used in the determination of these compounds. The work is structured as follows and affecting major analytical difficulties: Procurement and commercial availability of standard solutions. Stage of sample treatment. Chromatographic analysis. (Author) 19 refs.

Comparison of the acetyl bromide spectrophotometric method with other analytical lignin methods for determining lignin concentration in forage samples.

Science.gov (United States)

Fukushima, Romualdo S; Hatfield, Ronald D

2004-06-16

Present analytical methods to quantify lignin in herbaceous plants are not totally satisfactory. A spectrophotometric method, acetyl bromide soluble lignin (ABSL), has been employed to determine lignin concentration in a range of plant materials. In this work, lignin extracted with acidic dioxane was used to develop standard curves and to calculate the derived linear regression equation (slope equals absorptivity value or extinction coefficient) for determining the lignin concentration of respective cell wall samples. This procedure yielded lignin values that were different from those obtained with Klason lignin, acid detergent acid insoluble lignin, or permanganate lignin procedures. Correlations with in vitro dry matter or cell wall digestibility of samples were highest with data from the spectrophotometric technique. The ABSL method employing as standard lignin extracted with acidic dioxane has the potential to be employed as an analytical method to determine lignin concentration in a range of forage materials. It may be useful in developing a quick and easy method to predict in vitro digestibility on the basis of the total lignin content of a sample.

Role of analytical chemistry in the development of nuclear fuels

International Nuclear Information System (INIS)

Ramakumar, K.L.

2012-01-01

quality of the fabricated fuel conforms to the chemical specifications for the fuel laid down by the fuel designer. These specifications are worked out for the major and minor constituents which affect the fuel properties and hence its performance under conditions prevailing in an operating reactor. Nuclear reactor design incorporates detailed specifications of different systems, which must be satisfied for smooth and efficient functioning of the reactor. Fuel being the heart of the reactor, its chemical characterisation is an important component of this design. Both the fuel materials and finished fuel products are to be characterised for this purpose. Each fuel batch has to be subjected to comprehensive chemical quality control for trace constituents, stoichiometry and isotopic composition. Analytical methodology for chemical quality control measurements is described below under different sections depending on the nature of measurements. These are: (1) preparation of starting materials, (2) Sampling methodologies, (3) Dissolution of samples, (4) Thorium, uranium and plutonium content, (5) Isotopic composition (for fissile and fertile content), (6) Americium content, (7) Oxygen to metal ratio, (8) Trace metals determination, (9) Trace non-metals determination,(10) Total gas content, and (11) Moisture content in the case of oxide fuels. The signal contributions of analytical chemistry for nuclear fuel fabrication are enumerated in this paper. (author)

Gatlinburg conference: barometer of progress in analytical chemistry

International Nuclear Information System (INIS)

Shults, W.D.

1981-01-01

Much progress has been made in the field of analytical chemistry over the past twenty-five years. The AEC-ERDA-DOE family of laboratories contributed greatly to this progress. It is not surprising then to find a close correlation between program content of past Gatlinburg conferences and developments in analytical methodology. These conferences have proved to be a barometer of technical status

How Big of a Problem is Analytic Error in Secondary Analyses of Survey Data?

Directory of Open Access Journals (Sweden)

Brady T West

Full Text Available Secondary analyses of survey data collected from large probability samples of persons or establishments further scientific progress in many fields. The complex design features of these samples improve data collection efficiency, but also require analysts to account for these features when conducting analysis. Unfortunately, many secondary analysts from fields outside of statistics, biostatistics, and survey methodology do not have adequate training in this area, and as a result may apply incorrect statistical methods when analyzing these survey data sets. This in turn could lead to the publication of incorrect inferences based on the survey data that effectively negate the resources dedicated to these surveys. In this article, we build on the results of a preliminary meta-analysis of 100 peer-reviewed journal articles presenting analyses of data from a variety of national health surveys, which suggested that analytic errors may be extremely prevalent in these types of investigations. We first perform a meta-analysis of a stratified random sample of 145 additional research products analyzing survey data from the Scientists and Engineers Statistical Data System (SESTAT, which describes features of the U.S. Science and Engineering workforce, and examine trends in the prevalence of analytic error across the decades used to stratify the sample. We once again find that analytic errors appear to be quite prevalent in these studies. Next, we present several example analyses of real SESTAT data, and demonstrate that a failure to perform these analyses correctly can result in substantially biased estimates with standard errors that do not adequately reflect complex sample design features. Collectively, the results of this investigation suggest that reviewers of this type of research need to pay much closer attention to the analytic methods employed by researchers attempting to publish or present secondary analyses of survey data.

How Big of a Problem is Analytic Error in Secondary Analyses of Survey Data?

Science.gov (United States)

West, Brady T.; Sakshaug, Joseph W.; Aurelien, Guy Alain S.

2016-01-01

Secondary analyses of survey data collected from large probability samples of persons or establishments further scientific progress in many fields. The complex design features of these samples improve data collection efficiency, but also require analysts to account for these features when conducting analysis. Unfortunately, many secondary analysts from fields outside of statistics, biostatistics, and survey methodology do not have adequate training in this area, and as a result may apply incorrect statistical methods when analyzing these survey data sets. This in turn could lead to the publication of incorrect inferences based on the survey data that effectively negate the resources dedicated to these surveys. In this article, we build on the results of a preliminary meta-analysis of 100 peer-reviewed journal articles presenting analyses of data from a variety of national health surveys, which suggested that analytic errors may be extremely prevalent in these types of investigations. We first perform a meta-analysis of a stratified random sample of 145 additional research products analyzing survey data from the Scientists and Engineers Statistical Data System (SESTAT), which describes features of the U.S. Science and Engineering workforce, and examine trends in the prevalence of analytic error across the decades used to stratify the sample. We once again find that analytic errors appear to be quite prevalent in these studies. Next, we present several example analyses of real SESTAT data, and demonstrate that a failure to perform these analyses correctly can result in substantially biased estimates with standard errors that do not adequately reflect complex sample design features. Collectively, the results of this investigation suggest that reviewers of this type of research need to pay much closer attention to the analytic methods employed by researchers attempting to publish or present secondary analyses of survey data. PMID:27355817

SPIDIA-RNA: First external quality assessment for the pre-analytical phase of blood samples used for RNA based analyses

Czech Academy of Sciences Publication Activity Database

Pazzagli, M.; Malentacchi, F.; Simi, L.; Wyrich, R.; Guenther, K.; Hartmann, C.; Verderio, P.; Pizzamiglio, S.; Ciniselli, C.M.; Tichopád, Aleš; Kubista, Mikael; Gelmini, S.

2013-01-01

Roč. 59, č. 1 (2013), s. 20-31 ISSN 1046-2023 Institutional research plan: CEZ:AV0Z50520701 Keywords : Pre-analytical phase * RNA quality * Blood samples Subject RIV: EB - Genetics ; Molecular Biology Impact factor: 3.221, year: 2013

Ball assisted device for analytical surface sampling

Science.gov (United States)

ElNaggar, Mariam S; Van Berkel, Gary J; Covey, Thomas R

2015-11-03

A system for sampling a surface includes a sampling probe having a housing and a socket, and a rolling sampling sphere within the socket. The housing has a sampling fluid supply conduit and a sampling fluid exhaust conduit. The sampling fluid supply conduit supplies sampling fluid to the sampling sphere. The sampling fluid exhaust conduit has an inlet opening for receiving sampling fluid carried from the surface by the sampling sphere. A surface sampling probe and a method for sampling a surface are also disclosed.

Micro-Crater Laser Induced Breakdown Spectroscopy--an Analytical approach in metals samples

Energy Technology Data Exchange (ETDEWEB)

Piscitelli, Vincent [UCV- Laboratorio de Espectroscopia Laser, Caracas (Venezuela); Lawrence Berkeley National laboratory, Berkeley, US (United States); Gonzalez, Jhanis; Xianglei, Mao; Russo, Richard [Lawrence Berkeley National laboratory, Berkeley, US (United States); Fernandez, Alberto [UCV- Laboratorio de Espectroscopia Laser, Caracas (Venezuela)

2008-04-15

The laser ablation has been increasing its popularity like as technique of chemical analysis. This is due to its great potentiality in the analysis of solid samples. On the way to contributing to the development of the technique, we in this work studied the laser induced breakdown spectroscopy (LIBS) in conditions of micro ablation for future studies of coverings and micro crates analysis. Craters between 2 and 7 micrometers of diameter were made using an Nd-YAG nanosecond laser in their fundamental emission of 1064 nm. In order to create these craters we use an objective lens of long distance work and 0.45 of numerical aperture. The atomic emission versus the energy of the laser and its effect on the size of craters was study. We found that below 3 micrometers although there was evidence of material removal by the formation of a crater, it was no detectable atomic emission for our instruments. In order to try to understand this, curves of size of crater versus plasma temperature using the Boltzmann distribution graphs taking the Copper emission lines in the visible region were made. In addition calibration curves for Copper and aluminum were made in two different matrices; one of it was a Cu/Zn alloy and the other a Zinc Matrix. The atomic lines Cu I (521.78 nm) and Al I (396.15 nm) was used. From the Calibration curve the analytical limit of detection and other analytical parameters were obtained.

Analytical methodology for determination of the sulfate in vinasse samples; Metodologia analitica para a determinacao de sulfato em vinhoto

Energy Technology Data Exchange (ETDEWEB)

Prada, Silvio Miranda; Guekezian, Marcia; Suarez-Ilha, Maria Encarnacion V. [Sao Paulo Univ., SP (Brazil). Inst. de Quimica

1998-05-01

When sulfate is present in high concentrations, it acts as an inhibitor in the production of methane (Biogas Formation) in anaerobic biodigestion processes. In this way it is very important to know the sulfate concentration in vinasse samples before to make the biodigester design. A previous developed and indirect method (Anal. Chim. Acta. 1996, 329, 197), was used to determine sulfate in samples of vinasse, after previous treatments, done in order to eliminate organic matter with hydrogen peroxide 30% and concentrated nitric acid mixture (3:1), under heating. Interferent cationic ions were isolated by using ion exchange columns. The results obtained for some samples from Araraquara and Penapolis are here presented. The phosphate concentration was also determined. (author) 23 refs., 3 tabs.

Analytical evaluation of BEA zeolite for the pre-concentration of polycyclic aromatic hydrocarbons and their subsequent chromatographic analysis in water samples.

Science.gov (United States)

Wilson, Walter B; Costa, Andréia A; Wang, Huiyong; Dias, José A; Dias, Sílvia C L; Campiglia, Andres D

2012-07-06

The analytical performance of BEA - a commercial zeolite - is evaluated for the pre-concentration of fifteen Environmental Protection Agency - polycyclic aromatic hydrocarbons and their subsequent HPLC analysis in tap and lake water samples. The pre-concentration factors obtained with BEA have led to a method with excellent analytical figures of merit. One milliliter aliquots were sufficient to obtain excellent precision of measurements at the parts-per-trillion concentration level with relative standard deviations varying from 4.1% (dibenzo[a,h]anthracene) to 13.4% (pyrene). The limits of detection were excellent as well and varied between 1.1 (anthracene) and 49.9 ng L(-1) (indeno[1,2,3-cd]pyrene). The recovery values of all the studied compounds meet the criterion for regulated polycyclic aromatic hydrocarbons, which mandates relative standard deviations equal or lower than 25%. The small volume of organic solvents (100 μL per sample) and amount of BEA (2 mg per sample) makes sample pre-concentration environmentally friendly and cost effective. The extraction procedure is well suited for numerous samples as the small working volume (1 mL) facilitates the implementation of simultaneous sample extraction. These are attractive features when routine monitoring of numerous samples is contemplated. Copyright © 2012 Elsevier B.V. All rights reserved.

Sampling and sample processing in pesticide residue analysis.

Science.gov (United States)

Lehotay, Steven J; Cook, Jo Marie

2015-05-13

Proper sampling and sample processing in pesticide residue analysis of food and soil have always been essential to obtain accurate results, but the subject is becoming a greater concern as approximately 100 mg test portions are being analyzed with automated high-throughput analytical methods by agrochemical industry and contract laboratories. As global food trade and the importance of monitoring increase, the food industry and regulatory laboratories are also considering miniaturized high-throughput methods. In conjunction with a summary of the symposium "Residues in Food and Feed - Going from Macro to Micro: The Future of Sample Processing in Residue Analytical Methods" held at the 13th IUPAC International Congress of Pesticide Chemistry, this is an opportune time to review sampling theory and sample processing for pesticide residue analysis. If collected samples and test portions do not adequately represent the actual lot from which they came and provide meaningful results, then all costs, time, and efforts involved in implementing programs using sophisticated analytical instruments and techniques are wasted and can actually yield misleading results. This paper is designed to briefly review the often-neglected but crucial topic of sample collection and processing and put the issue into perspective for the future of pesticide residue analysis. It also emphasizes that analysts should demonstrate the validity of their sample processing approaches for the analytes/matrices of interest and encourages further studies on sampling and sample mass reduction to produce a test portion.

Pre-Analytical Considerations for Successful Next-Generation Sequencing (NGS: Challenges and Opportunities for Formalin-Fixed and Paraffin-Embedded Tumor Tissue (FFPE Samples

Directory of Open Access Journals (Sweden)

Gladys Arreaza

2016-09-01

Full Text Available In cancer drug discovery, it is important to investigate the genetic determinants of response or resistance to cancer therapy as well as factors that contribute to adverse events in the course of clinical trials. Despite the emergence of new technologies and the ability to measure more diverse analytes (e.g., circulating tumor cell (CTC, circulating tumor DNA (ctDNA, etc., tumor tissue is still the most common and reliable source for biomarker investigation. Because of its worldwide use and ability to preserve samples for many decades at ambient temperature, formalin-fixed, paraffin-embedded tumor tissue (FFPE is likely to be the preferred choice for tissue preservation in clinical practice for the foreseeable future. Multiple analyses are routinely performed on the same FFPE samples (such as Immunohistochemistry (IHC, in situ hybridization, RNAseq, DNAseq, TILseq, Methyl-Seq, etc.. Thus, specimen prioritization and optimization of the isolation of analytes is critical to ensure successful completion of each assay. FFPE is notorious for producing suboptimal DNA quality and low DNA yield. However, commercial vendors tend to request higher DNA sample mass than what is actually required for downstream assays, which restricts the breadth of biomarker work that can be performed. We evaluated multiple genomics service laboratories to assess the current state of NGS pre-analytical processing of FFPE. Significant differences in pre-analytical capabilities were observed. Key aspects are highlighted and recommendations are made to improve the current practice in translational research.

Pre-analytical and analytical variation of drug determination in segmented hair using ultra-performance liquid chromatography-tandem mass spectrometry.

Science.gov (United States)

Nielsen, Marie Katrine Klose; Johansen, Sys Stybe; Linnet, Kristian

2014-01-01

Assessment of total uncertainty of analytical methods for the measurements of drugs in human hair has mainly been derived from the analytical variation. However, in hair analysis several other sources of uncertainty will contribute to the total uncertainty. Particularly, in segmental hair analysis pre-analytical variations associated with the sampling and segmentation may be significant factors in the assessment of the total uncertainty budget. The aim of this study was to develop and validate a method for the analysis of 31 common drugs in hair using ultra-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) with focus on the assessment of both the analytical and pre-analytical sampling variations. The validated method was specific, accurate (80-120%), and precise (CV≤20%) across a wide linear concentration range from 0.025-25 ng/mg for most compounds. The analytical variation was estimated to be less than 15% for almost all compounds. The method was successfully applied to 25 segmented hair specimens from deceased drug addicts showing a broad pattern of poly-drug use. The pre-analytical sampling variation was estimated from the genuine duplicate measurements of two bundles of hair collected from each subject after subtraction of the analytical component. For the most frequently detected analytes, the pre-analytical variation was estimated to be 26-69%. Thus, the pre-analytical variation was 3-7 folds larger than the analytical variation (7-13%) and hence the dominant component in the total variation (29-70%). The present study demonstrated the importance of including the pre-analytical variation in the assessment of the total uncertainty budget and in the setting of the 95%-uncertainty interval (±2CVT). Excluding the pre-analytical sampling variation could significantly affect the interpretation of results from segmental hair analysis. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

Laser sampling

International Nuclear Information System (INIS)

Gorbatenko, A A; Revina, E I

2015-01-01

The review is devoted to the major advances in laser sampling. The advantages and drawbacks of the technique are considered. Specific features of combinations of laser sampling with various instrumental analytical methods, primarily inductively coupled plasma mass spectrometry, are discussed. Examples of practical implementation of hybrid methods involving laser sampling as well as corresponding analytical characteristics are presented. The bibliography includes 78 references

New approaches to wipe sampling methods for antineoplastic and other hazardous drugs in healthcare settings.

Science.gov (United States)

Connor, Thomas H; Smith, Jerome P

2016-09-01

At the present time, the method of choice to determine surface contamination of the workplace with antineoplastic and other hazardous drugs is surface wipe sampling and subsequent sample analysis with a variety of analytical techniques. The purpose of this article is to review current methodology for determining the level of surface contamination with hazardous drugs in healthcare settings and to discuss recent advances in this area. In addition it will provide some guidance for conducting surface wipe sampling and sample analysis for these drugs in healthcare settings. Published studies on the use of wipe sampling to measure hazardous drugs on surfaces in healthcare settings drugs were reviewed. These studies include the use of well-documented chromatographic techniques for sample analysis in addition to newly evolving technology that provides rapid analysis of specific antineoplastic. Methodology for the analysis of surface wipe samples for hazardous drugs are reviewed, including the purposes, technical factors, sampling strategy, materials required, and limitations. The use of lateral flow immunoassay (LFIA) and fluorescence covalent microbead immunosorbent assay (FCMIA) for surface wipe sample evaluation is also discussed. Current recommendations are that all healthc a re settings where antineoplastic and other hazardous drugs are handled include surface wipe sampling as part of a comprehensive hazardous drug-safe handling program. Surface wipe sampling may be used as a method to characterize potential occupational dermal exposure risk and to evaluate the effectiveness of implemented controls and the overall safety program. New technology, although currently limited in scope, may make wipe sampling for hazardous drugs more routine, less costly, and provide a shorter response time than classical analytical techniques now in use.

Reducing Conservatism of Analytic Transient Response Bounds via Shaping Filters

Science.gov (United States)

Kwan, Aiyueh; Bedrossian, Nazareth; Jan, Jiann-Woei; Grigoriadis, Karolos; Hua, Tuyen (Technical Monitor)

1999-01-01

Recent results show that the peak transient response of a linear system to bounded energy inputs can be computed using the energy-to-peak gain of the system. However, analytically computed peak response bound can be conservative for a class of class bounded energy signals, specifically pulse trains generated from jet firings encountered in space vehicles. In this paper, shaping filters are proposed as a Methodology to reduce the conservatism of peak response analytic bounds. This Methodology was applied to a realistic Space Station assembly operation subject to jet firings. The results indicate that shaping filters indeed reduce the predicted peak response bounds.

Supercritical fluid analytical methods

International Nuclear Information System (INIS)

Smith, R.D.; Kalinoski, H.T.; Wright, B.W.; Udseth, H.R.

1988-01-01

Supercritical fluids are providing the basis for new and improved methods across a range of analytical technologies. New methods are being developed to allow the detection and measurement of compounds that are incompatible with conventional analytical methodologies. Characterization of process and effluent streams for synfuel plants requires instruments capable of detecting and measuring high-molecular-weight compounds, polar compounds, or other materials that are generally difficult to analyze. The purpose of this program is to develop and apply new supercritical fluid techniques for extraction, separation, and analysis. These new technologies will be applied to previously intractable synfuel process materials and to complex mixtures resulting from their interaction with environmental and biological systems

Perspectives on making big data analytics work for oncology.

Science.gov (United States)

El Naqa, Issam

2016-12-01

Oncology, with its unique combination of clinical, physical, technological, and biological data provides an ideal case study for applying big data analytics to improve cancer treatment safety and outcomes. An oncology treatment course such as chemoradiotherapy can generate a large pool of information carrying the 5Vs hallmarks of big data. This data is comprised of a heterogeneous mixture of patient demographics, radiation/chemo dosimetry, multimodality imaging features, and biological markers generated over a treatment period that can span few days to several weeks. Efforts using commercial and in-house tools are underway to facilitate data aggregation, ontology creation, sharing, visualization and varying analytics in a secure environment. However, open questions related to proper data structure representation and effective analytics tools to support oncology decision-making need to be addressed. It is recognized that oncology data constitutes a mix of structured (tabulated) and unstructured (electronic documents) that need to be processed to facilitate searching and subsequent knowledge discovery from relational or NoSQL databases. In this context, methods based on advanced analytics and image feature extraction for oncology applications will be discussed. On the other hand, the classical p (variables)≫n (samples) inference problem of statistical learning is challenged in the Big data realm and this is particularly true for oncology applications where p-omics is witnessing exponential growth while the number of cancer incidences has generally plateaued over the past 5-years leading to a quasi-linear growth in samples per patient. Within the Big data paradigm, this kind of phenomenon may yield undesirable effects such as echo chamber anomalies, Yule-Simpson reversal paradox, or misleading ghost analytics. In this work, we will present these effects as they pertain to oncology and engage small thinking methodologies to counter these effects ranging from

16 Offsetting deficit conceptualisations: methodological ...

African Journals Online (AJOL)

uses the concepts of literacy practices and knowledge recontextualisation to ... 1996, 2000) theory of 'knowledge recontextualisation' in the development of curricula .... cognitive, social and cultural abilities needed to fit in and thrive in the HE learning .... this argument, that a methodology and analytic framework that seeks to ...

Analytical chemistry

Energy Technology Data Exchange (ETDEWEB)

Chae, Myeong Hu; Lee, Hu Jun; Kim, Ha Seok

1989-02-15

This book give explanations on analytical chemistry with ten chapters, which deal with development of analytical chemistry, the theory of error with definition and classification, sample and treatment gravimetry on general process of gravimetry in aqueous solution and non-aqueous solution, precipitation titration about precipitation reaction and types, complexometry with summary and complex compound, oxidation-reduction equilibrium on electrode potential and potentiometric titration, solvent extraction and chromatograph and experiment with basic operation for chemical experiment.

Analytical chemistry

International Nuclear Information System (INIS)

Chae, Myeong Hu; Lee, Hu Jun; Kim, Ha Seok

1989-02-01

This book give explanations on analytical chemistry with ten chapters, which deal with development of analytical chemistry, the theory of error with definition and classification, sample and treatment gravimetry on general process of gravimetry in aqueous solution and non-aqueous solution, precipitation titration about precipitation reaction and types, complexometry with summary and complex compound, oxidation-reduction equilibrium on electrode potential and potentiometric titration, solvent extraction and chromatograph and experiment with basic operation for chemical experiment.

ANALYTIC HIERARCHY PROCESS: AN APPLICATION IN GREEN BUILDING MARKET RESEARCH

Directory of Open Access Journals (Sweden)

Sharmin Attaran

2013-01-01

Full Text Available Sustainability has become a necessity in the building industry. In recent years, as the general public is more informed and aware of sustainability related issues, they are becoming major players in the decision making process regarding their built environment. However, there are still challenges with how sustainability is communicated to occupants and owners of buildings. As the global economic crisis is continuing, the marketing of green buildings needs to be refined to communicate the lifetime benefits of sustainability. One of the ways to develop effective marketing strategies, is to understand what the occupants value the most among many aspects of green buildings thus develop focused marketing solutions. Authors present a conceptual methodology using Analytic Hierarchy Process toward identifying consumer ranking and weights of a major green building rating system’s categories. Authors use sample non-representative data to illustrate the proposed methodology, while sharing preliminary qualitative data from the research in progress.

Determination of proline in honey: comparison between official methods, optimization and validation of the analytical methodology.

Science.gov (United States)

Truzzi, Cristina; Annibaldi, Anna; Illuminati, Silvia; Finale, Carolina; Scarponi, Giuseppe

2014-05-01

The study compares official spectrophotometric methods for the determination of proline content in honey - those of the International Honey Commission (IHC) and the Association of Official Analytical Chemists (AOAC) - with the original Ough method. Results show that the extra time-consuming treatment stages added by the IHC method with respect to the Ough method are pointless. We demonstrate that the AOACs method proves to be the best in terms of accuracy and time saving. The optimized waiting time for the absorbance recording is set at 35min from the removal of reaction tubes from the boiling bath used in the sample treatment. The optimized method was validated in the matrix: linearity up to 1800mgL(-1), limit of detection 20mgL(-1), limit of quantification 61mgL(-1). The method was applied to 43 unifloral honey samples from the Marche region, Italy. Copyright © 2013 Elsevier Ltd. All rights reserved.

A Progressive Approach to Teaching Analytics in the Marketing Curriculum

Science.gov (United States)

Liu, Yiyuan; Levin, Michael A.

2018-01-01

With the emerging use of analytics tools and methodologies in marketing, marketing educators have provided students training and experiences beyond the soft skills associated with understanding consumer behavior. Previous studies have only discussed how to apply analytics in course designs, tools, and related practices. However, there is a lack of…

Studies on application of neutron activation analysis -Applied research on air pollution monitoring and development of analytical method of environmental samples

International Nuclear Information System (INIS)

Chung, Yong Sam; Moon, Jong Hwa; Chung, Young Ju; Jeong, Eui Sik; Lee, Sang Mi; Kang, Sang Hun; Cho, Seung Yeon; Kwon, Young Sik; Chung, Sang Wuk; Lee, Kyu Sung; Chun, Ki Hong; Kim, Nak Bae; Lee, Kil Yong; Yoon, Yoon Yeol; Chun, Sang Ki.

1997-09-01

This research report is written for results of applied research on air pollution monitoring using instrumental neutron activation analysis. For identification and standardization of analytical method, 24 environmental samples are analyzed quantitatively, and accuracy and precision of this method are measured. Using airborne particulate matter and biomonitor chosen as environmental indicators, trace elemental concentrations of sample collected at urban and rural site monthly are determined ant then the calculation of statistics and the factor analysis are carried out for investigation of emission source. Facilities for NAA are installed in a new HANARO reactor, functional test is performed for routine operation. In addition, unified software code for NAA is developed to improve accuracy, precision and abilities of analytical processes. (author). 103 refs., 61 tabs., 19 figs

Implementing analytics a blueprint for design, development, and adoption

CERN Document Server

Sheikh, Nauman

2013-01-01

Implementing Analytics demystifies the concept, technology and application of analytics and breaks its implementation down to repeatable and manageable steps, making it possible for widespread adoption across all functions of an organization. Implementing Analytics simplifies and helps democratize a very specialized discipline to foster business efficiency and innovation without investing in multi-million dollar technology and manpower. A technology agnostic methodology that breaks down complex tasks like model design and tuning and emphasizes business decisions rather than the technology behi

Laboratory methodologies for indicators of iron status: strengths, limitations, and analytical challenges.

Science.gov (United States)

Pfeiffer, Christine M; Looker, Anne C

2017-12-01

Biochemical assessment of iron status relies on serum-based indicators, such as serum ferritin (SF), transferrin saturation, and soluble transferrin receptor (sTfR), as well as erythrocyte protoporphyrin. These indicators present challenges for clinical practice and national nutrition surveys, and often iron status interpretation is based on the combination of several indicators. The diagnosis of iron deficiency (ID) through SF concentration, the most commonly used indicator, is complicated by concomitant inflammation. sTfR concentration is an indicator of functional ID that is not an acute-phase reactant, but challenges in its interpretation arise because of the lack of assay standardization, common reference ranges, and common cutoffs. It is unclear which indicators are best suited to assess excess iron status. The value of hepcidin, non-transferrin-bound iron, and reticulocyte indexes is being explored in research settings. Serum-based indicators are generally measured on fully automated clinical analyzers available in most hospitals. Although international reference materials have been available for years, the standardization of immunoassays is complicated by the heterogeneity of antibodies used and the absence of physicochemical reference methods to establish "true" concentrations. From 1988 to 2006, the assessment of iron status in NHANES was based on the multi-indicator ferritin model. However, the model did not indicate the severity of ID and produced categorical estimates. More recently, iron status assessment in NHANES has used the total body iron stores (TBI) model, in which the log ratio of sTfR to SF is assessed. Together, sTfR and SF concentrations cover the full range of iron status. The TBI model better predicts the absence of bone marrow iron than SF concentration alone, and TBI can be analyzed as a continuous variable. Additional consideration of methodologies, interpretation of indicators, and analytic standardization is important for further

Supercritical fluid extraction and ultra performance liquid chromatography of respiratory quinones for microbial community analysis in environmental and biological samples.

Science.gov (United States)

Hanif, Muhammad; Atsuta, Yoichi; Fujie, Koichi; Daimon, Hiroyuki

2012-03-05

Microbial community structure plays a significant role in environmental assessment and animal health management. The development of a superior analytical strategy for the characterization of microbial community structure is an ongoing challenge. In this study, we developed an effective supercritical fluid extraction (SFE) and ultra performance liquid chromatography (UPLC) method for the analysis of bacterial respiratory quinones (RQ) in environmental and biological samples. RQ profile analysis is one of the most widely used culture-independent tools for characterizing microbial community structure. A UPLC equipped with a photo diode array (PDA) detector was successfully applied to the simultaneous determination of ubiquinones (UQ) and menaquinones (MK) without tedious pretreatment. Supercritical carbon dioxide (scCO(2)) extraction with the solid-phase cartridge trap proved to be a more effective and rapid method for extracting respiratory quinones, compared to a conventional organic solvent extraction method. This methodology leads to a successful analytical procedure that involves a significant reduction in the complexity and sample preparation time. Application of the optimized methodology to characterize microbial communities based on the RQ profile was demonstrated for a variety of environmental samples (activated sludge, digested sludge, and compost) and biological samples (swine and Japanese quail feces).

Model and Analytic Processes for Export License Assessments

Energy Technology Data Exchange (ETDEWEB)

Thompson, Sandra E.; Whitney, Paul D.; Weimar, Mark R.; Wood, Thomas W.; Daly, Don S.; Brothers, Alan J.; Sanfilippo, Antonio P.; Cook, Diane; Holder, Larry

2011-09-29

This paper represents the Department of Energy Office of Nonproliferation Research and Development (NA-22) Simulations, Algorithms and Modeling (SAM) Program's first effort to identify and frame analytical methods and tools to aid export control professionals in effectively predicting proliferation intent; a complex, multi-step and multi-agency process. The report focuses on analytical modeling methodologies that alone, or combined, may improve the proliferation export control license approval process. It is a follow-up to an earlier paper describing information sources and environments related to international nuclear technology transfer. This report describes the decision criteria used to evaluate modeling techniques and tools to determine which approaches will be investigated during the final 2 years of the project. The report also details the motivation for why new modeling techniques and tools are needed. The analytical modeling methodologies will enable analysts to evaluate the information environment for relevance to detecting proliferation intent, with specific focus on assessing risks associated with transferring dual-use technologies. Dual-use technologies can be used in both weapons and commercial enterprises. A decision-framework was developed to evaluate which of the different analytical modeling methodologies would be most appropriate conditional on the uniqueness of the approach, data availability, laboratory capabilities, relevance to NA-22 and Office of Arms Control and Nonproliferation (NA-24) research needs and the impact if successful. Modeling methodologies were divided into whether they could help micro-level assessments (e.g., help improve individual license assessments) or macro-level assessment. Macro-level assessment focuses on suppliers, technology, consumers, economies, and proliferation context. Macro-level assessment technologies scored higher in the area of uniqueness because less work has been done at the macro level. An

An Analytic Framework for the War of Ideas

National Research Council Canada - National Science Library

Schramm, Harrison C

2006-01-01

...." This thesis seeks to place an analytic framework around this war. The goal is to create a methodology for considering alternatives and some concrete metrics with which to compare courses of action...

Sample preparation prior to the LC-MS-based metabolomics/metabonomics of blood-derived samples.

Science.gov (United States)

Gika, Helen; Theodoridis, Georgios

2011-07-01

Blood represents a very important biological fluid and has been the target of continuous and extensive research for diagnostic, or health and drug monitoring reasons. Recently, metabonomics/metabolomics have emerged as a new and promising 'omics' platform that shows potential in biomarker discovery, especially in areas such as disease diagnosis, assessment of drug efficacy or toxicity. Blood is collected in various establishments in conditions that are not standardized. Next, the samples are prepared and analyzed using different methodologies or tools. When targeted analysis of key molecules (e.g., a drug or its metabolite[s]) is the aim, enforcement of certain measures or additional analyses may correct and harmonize these discrepancies. In omics fields such as those performed by holistic analytical approaches, no such rules or tools are available. As a result, comparison or correlation of results or data fusion becomes impractical. However, it becomes evident that such obstacles should be overcome in the near future to allow for large-scale studies that involve the assaying of samples from hundreds of individuals. In this case the effect of sample handling and preparation becomes very serious, in order to avoid wasting months of work from experts and expensive instrument time. The present review aims to cover the different methodologies applied to the pretreatment of blood prior to LC-MS metabolomic/metabonomic studies. The article tries to critically compare the methods and highlight issues that need to be addressed.

The analytical utility of thermally desorbed polydimethylsilicone membranes for in-vivo sampling of volatile organic compounds in and on human skin.

Science.gov (United States)

Riazanskaia, S; Blackburn, G; Harker, M; Taylor, D; Thomas, C L P

2008-08-01

A thermally-desorbed polydimethylsilicone (PDMS) membrane approach with analysis by gas chromatography-mass spectrometry has been developed and characterised, to enable the VOC arising in, and on skin, from glandular secretions, exogenous materials, products of perfusion from blood, and microbiological metabolites to be sampled in a single procedure. In-vitro studies using a series of volatile fatty acid standards indicated that the recovery efficiency of the technique increased with decreasing volatility; for example, the recovery of hexanoic acid was 3.3 times greater than that for 2-methylpropanoic acid. The relative standard deviation of the methodology decreased with decreasing volatility; RSD = 19% for 2-methylpropanoic acid and RSD = 7% for hexanoic acid. Sampled-mass vs. response relationships were modelled satisfactorily using linear regression analysis with regression coefficients in the range 0.95 to 0.998. In-vivo reproducibility was assessed though the analysis of the responses of 1-dodecane, 3,7-dimethyloct-1-ene, 2-propenoic acid, 2-ethylhexyl ester, 2-ethylhexan-1-ol, butanoic, 2-ethylhexylester, and junipen (1,4-methanoazulene, decahydro-4,8,8-trimethyl-9-methylene-); six compounds selected at random retention times from a GC-MS chromatographic VOC profile of human skin containing several hundred resolved and partially resolved compounds. Five samples were obtained simultaneously from the forearm of a healthy male participant. The in-vivo sample masses were estimated to be in the range 50 pg to 100 ng per sample with observed RSD falling between 15% and 32%; in line with a Horwitz trend. Increasing the sample time from 5 min to 120 min generally resulted in an enrichment of the VOC recovered, and for many VOC substantial increases in sensitivity (x7) were observed over this time range as the PDMS sampling-patch approached equilibrium with the underlying skin. Nevertheless, more volatile components, 2,4,6-trimethylcarbazole for instance, were

Is a pre-analytical process for urinalysis required?

Science.gov (United States)

Petit, Morgane; Beaudeux, Jean-Louis; Majoux, Sandrine; Hennequin, Carole

2017-10-01

For the reliable urinary measurement of calcium, phosphate and uric acid, a pre-analytical process by adding acid or base to urine samples at laboratory is recommended in order to dissolve precipitated solutes. Several studies on different kind of samples and analysers have previously shown that a such pre-analytical treatment is useless. The objective was to study the necessity of pre-analytical treatment of urine on samples collected using the V-Monovette ® (Sarstedt) system and measured on the analyser Architect C16000 (Abbott Diagnostics). Sixty urinary samples of hospitalized patients were selected (n=30 for calcium and phosphate, and n=30 for uric acid). After acidification of urine samples for measurement of calcium and phosphate, and alkalinisation for measurement of uric acid respectively, differences between results before and after the pre-analytical treatment were compared to acceptable limits recommended by the French society of clinical biology (SFBC). No difference in concentration between before and after pre-analytical treatment of urine samples exceeded acceptable limits from SFBC for measurement of calcium and uric acid. For phosphate, only one sample exceeded these acceptable limits, showing a result paradoxically lower after acidification. In conclusion, in agreement with previous study, our results show that acidification or alkalinisation of urine samples from 24 h urines or from urination is not a pre-analytical necessity for measurement of calcium, phosphate and uric acid.

A review of analytical procedures for the simultaneous determination of medically important veterinary antibiotics in environmental water: Sample preparation, liquid chromatography, and mass spectrometry.

Science.gov (United States)

Kim, Chansik; Ryu, Hong-Duck; Chung, Eu Gene; Kim, Yongseok; Lee, Jae-Kwan

2018-07-01

Medically important (MI) antibiotics are defined by the United States Food and Drug Administration as drugs containing certain active antimicrobial ingredients that are used for the treatment of human diseases or enteric pathogens causing food-borne diseases. The presence of MI antibiotic residues in environmental water is a major concern for both aquatic ecosystems and public health, particularly because of their potential to contribute to the development of antimicrobial-resistant microorganisms. In this article, we present a review of global trends in the sales of veterinary MI antibiotics and the analytical methodologies used for the simultaneous determination of antibiotic residues in environmental water. According to recently published government reports, sales volumes have increased steadily, despite many countries having adopted strategies for reducing the consumption of antibiotics. Global attention needs to be directed urgently at establishing new management strategies for reducing the use of MI antimicrobial products in the livestock industry. The development of standardized analytical methods for the detection of multiple residues is required to monitor and understand the fate of antibiotics in the environment. Simultaneous analyses of antibiotics have mostly been conducted using high-performance liquid chromatography-tandem mass spectrometry with a solid-phase extraction (SPE) pretreatment step. Currently, on-line SPE protocols are used for the rapid and sensitive detection of antibiotics in water samples. On-line detection protocols must be established for the monitoring and screening of unknown metabolites and transformation products of antibiotics in environmental water. Copyright © 2018 Elsevier Ltd. All rights reserved.

User-Centered Evaluation of Visual Analytics

Energy Technology Data Exchange (ETDEWEB)

Scholtz, Jean C.

2017-10-01

Visual analytics systems are becoming very popular. More domains now use interactive visualizations to analyze the ever-increasing amount and heterogeneity of data. More novel visualizations are being developed for more tasks and users. We need to ensure that these systems can be evaluated to determine that they are both useful and usable. A user-centered evaluation for visual analytics needs to be developed for these systems. While many of the typical human-computer interaction (HCI) evaluation methodologies can be applied as is, others will need modification. Additionally, new functionality in visual analytics systems needs new evaluation methodologies. There is a difference between usability evaluations and user-centered evaluations. Usability looks at the efficiency, effectiveness, and user satisfaction of users carrying out tasks with software applications. User-centered evaluation looks more specifically at the utility provided to the users by the software. This is reflected in the evaluations done and in the metrics used. In the visual analytics domain this is very challenging as users are most likely experts in a particular domain, the tasks they do are often not well defined, the software they use needs to support large amounts of different kinds of data, and often the tasks last for months. These difficulties are discussed more in the section on User-centered Evaluation. Our goal is to provide a discussion of user-centered evaluation practices for visual analytics, including existing practices that can be carried out and new methodologies and metrics that need to be developed and agreed upon by the visual analytics community. The material provided here should be of use for both researchers and practitioners in the field of visual analytics. Researchers and practitioners in HCI and interested in visual analytics will find this information useful as well as a discussion on changes that need to be made to current HCI practices to make them more suitable to

Determination of uranium in ground water using different analytical techniques

International Nuclear Information System (INIS)

Sahu, S.K.; Maity, Sukanta; Bhangare, R.C.; Pandit, G.G.; Sharma, D.N.

2014-10-01

The concern over presence of natural radionuclides like uranium in drinking water is growing recently. The contamination of aquifers with radionuclides depends on number of factors. The geology of an area is the most important factor along with anthropogenic activities like mining, coal ash disposal from thermal power plants, use of phosphate fertilizers etc. Whatever may be the source, the presence of uranium in drinking waters is a matter of great concern for public health. Studies show that uranium is a chemo-toxic and nephrotoxic heavy metal. This chemotoxicity affects the kidneys and bones in particular. Seeing the potential health hazards from natural radionuclides in drinking water, many countries worldwide have adopted the guideline activity concentration for drinking water quality recommended by the WHO (2011). For uranium, WHO has set a limit of 30μgL-1 in drinking water. The geological distribution of uranium and its migration in environment is of interest because the element is having environmental and exposure concerns. It is of great interest to use an analytical technique for uranium analysis in water which is highly sensitive especially at trace levels, specific and precise in presence of other naturally occurring major and trace metals and needs small amount of sample. Various analytical methods based on the use of different techniques have been developed in the past for the determination of uranium in the geological samples. The determination of uranium requires high selectivity due to its strong association with other elements. Several trace level wet chemistry analytical techniques have been reported for uranium determination, but most of these involve tedious and pain staking procedures, high detection limits, interferences etc. Each analytical technique has its own merits and demerits. Comparative assessment by different techniques can provide better quality control and assurance. In present study, uranium was analysed in ground water samples

Educational design as conversation : A conversation analytical perspective on teacher dialogue

NARCIS (Netherlands)

van Kruiningen, Jacqueline F.

The aim of this methodological paper is to expound on and demonstrate the value of conversation-analytical research in the area of (informal) teacher learning. The author discusses some methodological issues in current research on interaction in teacher learning and holds a plea for

Analytical Chemistry Division annual progress report for period ending November 30, 1977

International Nuclear Information System (INIS)

Lyon, W.S.

1978-03-01

Activities for the year are summarized in sections on analytical methodology, mass and mass emission spectrometry, analytical services, bio-organic analysis, nuclear and radiochemical analysis, and quality assurance and safety. Presentations of research results in publications and reports are tabulated

Analytical Chemistry Division annual progress report for period ending November 30, 1977

Energy Technology Data Exchange (ETDEWEB)

Lyon, W.S. (ed.)

1978-03-01

Activities for the year are summarized in sections on analytical methodology, mass and mass emission spectrometry, analytical services, bio-organic analysis, nuclear and radiochemical analysis, and quality assurance and safety. Presentations of research results in publications and reports are tabulated. (JRD)

Use of CTX-I and PINP as bone turnover markers: National Bone Health Alliance recommendations to standardize sample handling and patient preparation to reduce pre-analytical variability.

Science.gov (United States)

Szulc, P; Naylor, K; Hoyle, N R; Eastell, R; Leary, E T

2017-09-01

The National Bone Health Alliance (NBHA) recommends standardized sample handling and patient preparation for C-terminal telopeptide of type I collagen (CTX-I) and N-terminal propeptide of type I procollagen (PINP) measurements to reduce pre-analytical variability. Controllable and uncontrollable patient-related factors are reviewed to facilitate interpretation and minimize pre-analytical variability. The IOF and the International Federation of Clinical Chemistry (IFCC) Bone Marker Standards Working Group have identified PINP and CTX-I in blood to be the reference markers of bone turnover for the fracture risk prediction and monitoring of osteoporosis treatment. Although used in clinical research for many years, bone turnover markers (BTM) have not been widely adopted in clinical practice primarily due to their poor within-subject and between-lab reproducibility. The NBHA Bone Turnover Marker Project team aim to reduce pre-analytical variability of CTX-I and PINP measurements through standardized sample handling and patient preparation. Recommendations for sample handling and patient preparations were made based on review of available publications and pragmatic considerations to reduce pre-analytical variability. Controllable and un-controllable patient-related factors were reviewed to facilitate interpretation and sample collection. Samples for CTX-I must be collected consistently in the morning hours in the fasted state. EDTA plasma is preferred for CTX-I for its greater sample stability. Sample collection conditions for PINP are less critical as PINP has minimal circadian variability and is not affected by food intake. Sample stability limits should be observed. The uncontrollable aspects (age, sex, pregnancy, immobility, recent fracture, co-morbidities, anti-osteoporotic drugs, other medications) should be considered in BTM interpretation. Adopting standardized sample handling and patient preparation procedures will significantly reduce controllable pre-analytical

[The methodology and sample description of the National Survey on Addiction Problems in Hungary 2015 (NSAPH 2015)].

Science.gov (United States)

Paksi, Borbala; Demetrovics, Zsolt; Magi, Anna; Felvinczi, Katalin

2017-06-01

This paper introduces the methods and methodological findings of the National Survey on Addiction Problems in Hungary (NSAPH 2015). Use patterns of smoking, alcohol use and other psychoactive substances were measured as well as that of certain behavioural addictions (problematic gambling - PGSI, DSM-V, eating disorders - SCOFF, problematic internet use - PIUQ, problematic on-line gaming - POGO, problematic social media use - FAS, exercise addictions - EAI-HU, work addiction - BWAS, compulsive buying - CBS). The paper describes the applied measurement techniques, sample selection, recruitment of respondents and the data collection strategy as well. Methodological results of the survey including reliability and validity of the measures are reported. The NSAPH 2015 research was carried out on a nationally representative sample of the Hungarian adult population aged 16-64 yrs (gross sample 2477, net sample 2274 persons) with the age group of 18-34 being overrepresented. Statistical analysis of the weight-distribution suggests that weighting did not create any artificial distortion in the database leaving the representativeness of the sample unaffected. The size of the weighted sample of the 18-64 years old adult population is 1490 persons. The extent of the theoretical margin of error in the weighted sample is ±2,5%, at a reliability level of 95% which is in line with the original data collection plans. Based on the analysis of reliability and the extent of errors beyond sampling within the context of the database we conclude that inconsistencies create relatively minor distortions in cumulative prevalence rates; consequently the database makes possible the reliable estimation of risk factors related to different substance use behaviours. The reliability indexes of measurements used for prevalence estimates of behavioural addictions proved to be appropriate, though the psychometric features in some cases suggest the presence of redundant items. The comparison of

Multiresidual determination of pesticides in agricultural soil sample using Quechers extraction methodology

International Nuclear Information System (INIS)

Castro Garcia, Consuelo del Pilar

2011-01-01

To achieve a sustainable agricultural production there are used different organic and inorganic products, among them we found the fertilizers and pesticides. When they are applied most of the product falls to the ground, generating significant sources of pollution in the areas near the application and depending on the mobility of the pesticide, it can reach more remote areas. That is why it is important to determine the pesticide residues in soil after their application, being the selection of the extraction method crucial for the subsequent traces detection. In the present work there was evaluated the QUECHERS extraction technique, a method used in food but modified for a different and complex matrix like soil in order to achieve acceptable efficiencies multi-residue extraction of 20 pesticides and their subsequent determination by gas chromatography with electron capture and mass detection. The method was applied for the determination of pesticides in three soil samples from an agricultural site with different slopes between them. The Results indicated that 75% of the pesticides tested had acceptable efficiencies, thus meeting the objective of achieving multiresidue determination of pesticides in agricultural soil samples by extraction methodology QUECHERS. Besides, the presence of the fungicide penconazole was only detected in the three samples, being the highest concentration of pesticide found in the area with less slope (V_A_B_A_J_O) (author)

FASP, an analytic resource appraisal program for petroleum play analysis

Science.gov (United States)

Crovelli, R.A.; Balay, R.H.

1986-01-01

An analytic probabilistic methodology for resource appraisal of undiscovered oil and gas resources in play analysis is presented in a FORTRAN program termed FASP. This play-analysis methodology is a geostochastic system for petroleum resource appraisal in explored as well as frontier areas. An established geologic model considers both the uncertainty of the presence of the assessed hydrocarbon and its amount if present. The program FASP produces resource estimates of crude oil, nonassociated gas, dissolved gas, and gas for a geologic play in terms of probability distributions. The analytic method is based upon conditional probability theory and many laws of expectation and variance. ?? 1986.

Concrete crushing and sampling, a methodology and technology for the unconditional release of concrete material from decommissioning

International Nuclear Information System (INIS)

Gills, R.; Lewandowski, P.; Ooms, B.; Reusen, N.; Van Laer, W.; Walthery, R.

2007-01-01

Belgoprocess started the industrial decommissioning of the main process building of the former Eurochemic reprocessing plant in 1990, after completion of a pilot project. Two small storage buildings for final products from reprocessing were dismantled to verify the assumptions made in a previous paper study on decommissioning, to demonstrate and develop dismantling techniques and to train personnel. Both buildings were emptied and decontaminated to background levels. They were demolished and the remaining concrete debris was disposed of as industrial waste and green field conditions restored. Currently, the decommissioning operations carried out at the main building have made substantial progress. They are executed on an industrial scale. In view of the final demolition of the building, foreseen to start in the middle of 2008, a clearance methodology for the concrete from the cells into the Eurochemic building has been developed. It considers at least one complete measurement of all concrete structures and the removal of all detected residual radionuclides. This monitoring sequence is followed by a controlled demolition of the concrete structures and crushing of the resulting concrete parts to smaller particles. During the crushing operations, metal parts are separated from the concrete and representative concrete samples are taken. The frequency of sampling meets the prevailing standards. In a further step, the concrete samples are milled, homogenised, and a smaller fraction is sent to the laboratory for analyses. The paper describes the developed concrete crushing and sampling methodology. (authors)

Copper and tin isotopic analysis of ancient bronzes for archaeological investigation: development and validation of a suitable analytical methodology.

Science.gov (United States)

Balliana, Eleonora; Aramendía, Maite; Resano, Martin; Barbante, Carlo; Vanhaecke, Frank

2013-03-01

Although in many cases Pb isotopic analysis can be relied on for provenance determination of ancient bronzes, sometimes the use of "non-traditional" isotopic systems, such as those of Cu and Sn, is required. The work reported on in this paper aimed at revising the methodology for Cu and Sn isotope ratio measurements in archaeological bronzes via optimization of the analytical procedures in terms of sample pre-treatment, measurement protocol, precision, and analytical uncertainty. For Cu isotopic analysis, both Zn and Ni were investigated for their merit as internal standard (IS) relied on for mass bias correction. The use of Ni as IS seems to be the most robust approach as Ni is less prone to contamination, has a lower abundance in bronzes and an ionization potential similar to that of Cu, and provides slightly better reproducibility values when applied to NIST SRM 976 Cu isotopic reference material. The possibility of carrying out direct isotopic analysis without prior Cu isolation (with AG-MP-1 anion exchange resin) was investigated by analysis of CRM IARM 91D bronze reference material, synthetic solutions, and archaeological bronzes. Both procedures (Cu isolation/no Cu isolation) provide similar δ (65)Cu results with similar uncertainty budgets in all cases (±0.02-0.04 per mil in delta units, k = 2, n = 4). Direct isotopic analysis of Cu therefore seems feasible, without evidence of spectral interference or matrix-induced effect on the extent of mass bias. For Sn, a separation protocol relying on TRU-Spec anion exchange resin was optimized, providing a recovery close to 100 % without on-column fractionation. Cu was recovered quantitatively together with the bronze matrix with this isolation protocol. Isotopic analysis of this Cu fraction provides δ (65)Cu results similar to those obtained upon isolation using AG-MP-1 resin. This means that Cu and Sn isotopic analysis of bronze alloys can therefore be carried out after a single chromatographic

Exploring the Design Space of Immersive Urban Analytics

OpenAIRE

Chen, Zhutian; Wang, Yifang; Sun, Tianchen; Gao, Xiang; Chen, Wei; Pan, Zhigeng; Qu, Huamin; Wu, Yingcai

2017-01-01

Recent years have witnessed the rapid development and wide adoption of immersive head-mounted devices, such as HTC VIVE, Oculus Rift, and Microsoft HoloLens. These immersive devices have the potential to significantly extend the methodology of urban visual analytics by providing critical 3D context information and creating a sense of presence. In this paper, we propose an theoretical model to characterize the visualizations in immersive urban analytics. Further more, based on our comprehensiv...

Matrix effects break the LC behavior rule for analytes in LC-MS/MS analysis of biological samples.

Science.gov (United States)

Fang, Nianbai; Yu, Shanggong; Ronis, Martin Jj; Badger, Thomas M

2015-04-01

High-performance liquid chromatography (HPLC) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) are generally accepted as the preferred techniques for detecting and quantitating analytes of interest in biological matrices on the basis of the rule that one chemical compound yields one LC-peak with reliable retention time (Rt.). However, in the current study, we have found that under the same LC-MS conditions, the Rt. and shape of LC-peaks of bile acids in urine samples from animals fed dissimilar diets differed significantly among each other. To verify this matrix effect, 17 authentic bile acid standards were dissolved in pure methanol or in methanol containing extracts of urine from pigs consuming either breast milk or infant formula and analyzed by LC-MS/MS. The matrix components in urine from piglets fed formula significantly reduced the LC-peak Rt. and areas of bile acids. This is the first characterization of this matrix effect on Rt. in the literature. Moreover, the matrix effect resulted in an unexpected LC behavior: one single compound yielded two LC-peaks, which broke the rule of one LC-peak for one compound. The three bile acid standards which exhibited this unconventional LC behavior were chenodeoxycholic acid, deoxycholic acid, and glycocholic acid. One possible explanation for this effect is that some matrix components may have loosely bonded to analytes, which changed the time analytes were retained on a chromatography column and interfered with the ionization of analytes in the MS ion source to alter the peak area. This study indicates that a comprehensive understanding of matrix effects is needed towards improving the use of HPLC and LC-MS/MS techniques for qualitative and quantitative analyses of analytes in pharmacokinetics, proteomics/metabolomics, drug development, and sports drug testing, especially when LC-MS/MS data are analyzed by automation software where identification of an analyte is based on its exact molecular weight and Rt

Analysis of water and soil from the wetlands of Upper Three Runs Creek. Volume 2A, Analytical data packages September--October 1991 sampling

Energy Technology Data Exchange (ETDEWEB)

Haselow, L.A.; Rogers, V.A. [Westinghouse Savannah River Co., Aiken, SC (United States); Riordan, C.J. [Metcalf and Eddy, Inc. (United States); Eidson, G.W.; Herring, M.K. [Normandeau Associates, Inc. (United States)

1992-08-01

Shallow water and soils along Upper Three Runs Creek (UTRC) and associated wetlands between SRS Road F and Cato Road were sampled for nonradioactive and radioactive constituents. The sampling program is associated with risk evaluations being performed for various regulatory documents in these areas of the Savannah River Site (SRS). WSRC selected fifty sampling sites bordering the Mixed Waste Management Facility (MWMF), F- and H-Area Seepage Basins (FHSB), and the Sanitary Landfill (SL). The analytical results from this study provided information on the water and soil quality in UTRC and its associated wetlands. The analytical results from this investigation indicated that the primary constituents and radiological indicators detected in the shallow water and soils were tritium, gross alpha, radium 226, total radium and strontium 90. This investigation involved the collection of shallow water samples during the Fall of 1991 and the Spring of 1992 at fifty (50) sampling locations. Sampling was performed during these periods to incorporate high and low water table periods. Samples were collected from three sections along UTRC denoted as Phase I (MWMF), Phase II (FHSB) and Phase III (SL). One vibracored soil sample was also collected in each phase during the Fall of 1991. This document is compiled solely of experimental data obtained from the sampling procedures.

Analysis of water and soil from the wetlands of Upper Three Runs Creek. Volume 2B: Analytical data packages, January--February 1992 sampling

Energy Technology Data Exchange (ETDEWEB)

Haselow, L.A.; Rogers, V.A. [Westinghouse Savannah River Co., Aiken, SC (United States); Riordan, C.J. [Metcalf and Eddy (United States); Eidson, G.W.; Herring, M.K. [Normandeau Associates, Inc., Aiken, SC (United States)

1992-08-01

Shallow water and soils along Upper Three Runs Creek (UTRC) and associated wetlands between SRS Road F and Cato Road were sampled for nonradioactive and radioactive constituents. The sampling program is associated with risk evaluations being performed for various regulatory documents in these areas of the Savannah River Site (SRS). WSRC selected fifty sampling sites bordering the Mixed Waste Management Facility (MWMF), F- and H-Area Seepage Basins (FHSB), and the Sanitary Landfill (SL). The analytical results from this study provided information on the water and soil quality in UTRC and its associated wetlands. The analytical results from this investigation indicated that the primary constituents and radiological indicators detected in the shallow water and soils were tritium, gross alpha, radium 226, total radium and strontium 90. This investigation involved the collection of shallow water samples during the Fall of 1991 and the Spring of 1992 at fifty (50) sampling locations. Sampling was performed during these periods to incorporate high and low water table periods. Samples were collected from three sections along UTRC denoted as Phase I (MWMF), Phase II (FHSB) and Phase III (SL). One vibracored soil sample was also collected in each phase during the Fall of 1991. This document is compiled of experimental data obtained from the sampling procedures.

Evaluation of the analytic performance of laboratories: inter-laboratorial study of the spectroscopy of atomic absorption

International Nuclear Information System (INIS)

Wong Wong, S. M.

1996-01-01

The author made an inter-laboratorial study, with the participation of 18 national laboratories, that have spectrophotometer of atomic absorption. To evaluate the methods of analysis of lead, sodium, potasium, calcium, magnesium, zinc, copper, manganese, and iron, in the ambit of mg/l. The samples, distributed in four rounds to the laboratories, were prepared from primary patterns, deionized and distilled water. The study evaluated the homogeneity and stability, and verified its concentration, using as a reference method, the spectrometry method of Inductively Coupled Plasma emission (1CP). To obtain the characteristics of analytic performance, it applied the norm ASTM E 691. To evaluated the analytic performance, it used harmonized protocol of the International Union of Pure and applied chemistry (IUPAC). The study obtained the 29% of the laboratories had a satisfactory analytic performance, 9% had a questionable performance and 62% made an unsatisfactory analytic performance, according to the IUPAC norm. The results of the values of the characteristic performance method, show that there is no intercomparability between the laboratories, which is attributed to the different methodologies of analysis. (S. Grainger)

Analytical Validation of a New Enzymatic and Automatable Method for d-Xylose Measurement in Human Urine Samples

Directory of Open Access Journals (Sweden)

Israel Sánchez-Moreno

2017-01-01

Full Text Available Hypolactasia, or intestinal lactase deficiency, affects more than half of the world population. Currently, xylose quantification in urine after gaxilose oral administration for the noninvasive diagnosis of hypolactasia is performed with the hand-operated nonautomatable phloroglucinol reaction. This work demonstrates that a new enzymatic xylose quantification method, based on the activity of xylose dehydrogenase from Caulobacter crescentus, represents an excellent alternative to the manual phloroglucinol reaction. The new method is automatable and facilitates the use of the gaxilose test for hypolactasia diagnosis in the clinical practice. The analytical validation of the new technique was performed in three different autoanalyzers, using buffer or urine samples spiked with different xylose concentrations. For the comparison between the phloroglucinol and the enzymatic assays, 224 urine samples of patients to whom the gaxilose test had been prescribed were assayed by both methods. A mean bias of −16.08 mg of xylose was observed when comparing the results obtained by both techniques. After adjusting the cut-off of the enzymatic method to 19.18 mg of xylose, the Kappa coefficient was found to be 0.9531, indicating an excellent level of agreement between both analytical procedures. This new assay represents the first automatable enzymatic technique validated for xylose quantification in urine.

Integrated sampling and analysis plan for samples measuring >10 mrem/hour

International Nuclear Information System (INIS)

Haller, C.S.

1992-03-01

This integrated sampling and analysis plan was prepared to assist in planning and scheduling of Hanford Site sampling and analytical activities for all waste characterization samples that measure greater than 10 mrem/hour. This report also satisfies the requirements of the renegotiated Interim Milestone M-10-05 of the Hanford Federal Facility Agreement and Consent Order (the Tri-Party Agreement). For purposes of comparing the various analytical needs with the Hanford Site laboratory capabilities, the analytical requirements of the various programs were normalized by converting required laboratory effort for each type of sample to a common unit of work, the standard analytical equivalency unit (AEU). The AEU approximates the amount of laboratory resources required to perform an extensive suite of analyses on five core segments individually plus one additional suite of analyses on a composite sample derived from a mixture of the five core segments and prepare a validated RCRA-type data package

Determination of biomass burning tracers in air samples by GC/MS

Science.gov (United States)

Janoszka, Katarzyna

2018-01-01

Levoglucosan (LG) as a main cellulose burning product at 300°C is a biomass burning tracer. LG characterize by relatively high molar mass and it is sorbed by particulate matter. In the study of air pollution monitoring LG is mainly analyzed in particulate matter, PM1 and PM2,5. The tracer create relatively high O-H…O bond and weaker C-H…O bond. Due to the hydrogen bond, LG dissolves very well in water. Analytical procedure of LG determination include: extraction, derivatization and analysis by gas chromatography coupled with mass spectrometry detector. In water samples levoglucosan is determined by liquid chromatography. The paper presents a methodology for particulate matter samples determination their analysis by gas chromatography coupled with a mass spectrometry detector. Determination of LG content in particulate matter was performed according to an analytical method based on simultaneous pyridine extraction and derivatization using N,O-bis (trimethylsilyl) trifluoroacetamide and trimethylchlorosilane mixture (BSTFA: TMCS, 99: 1).

Determination of biomass burning tracers in air samples by GC/MS

Directory of Open Access Journals (Sweden)

Janoszka Katarzyna

2018-01-01

Full Text Available Levoglucosan (LG as a main cellulose burning product at 300°C is a biomass burning tracer. LG characterize by relatively high molar mass and it is sorbed by particulate matter. In the study of air pollution monitoring LG is mainly analyzed in particulate matter, PM1 and PM2,5. The tracer create relatively high O-H…O bond and weaker C-H…O bond. Due to the hydrogen bond, LG dissolves very well in water. Analytical procedure of LG determination include: extraction, derivatization and analysis by gas chromatography coupled with mass spectrometry detector. In water samples levoglucosan is determined by liquid chromatography. The paper presents a methodology for particulate matter samples determination their analysis by gas chromatography coupled with a mass spectrometry detector. Determination of LG content in particulate matter was performed according to an analytical method based on simultaneous pyridine extraction and derivatization using N,O-bis (trimethylsilyl trifluoroacetamide and trimethylchlorosilane mixture (BSTFA: TMCS, 99: 1.

The NLC Software Requirements Methodology

Energy Technology Data Exchange (ETDEWEB)

Shoaee, Hamid

2002-08-20

We describe the software requirements and development methodology developed for the NLC control system. Given the longevity of that project, and the likely geographical distribution of the collaborating engineers, the planned requirements management process is somewhat more formal than the norm in high energy physics projects. The short term goals of the requirements process are to accurately estimate costs, to decompose the problem, and to determine likely technologies. The long term goal is to enable a smooth transition from high level functional requirements to specific subsystem and component requirements for individual programmers, and to support distributed development. The methodology covers both ends of that life cycle. It covers both the analytical and documentary tools for software engineering, and project management support. This paper introduces the methodology, which is fully described in [1].

Speciated arsenic in air: measurement methodology and risk assessment considerations.

Science.gov (United States)

Lewis, Ari S; Reid, Kim R; Pollock, Margaret C; Campleman, Sharan L

2012-01-01

Accurate measurement of arsenic (As) in air is critical to providing a more robust understanding of arsenic exposures and associated human health risks. Although there is extensive information available on total arsenic in air, less is known on the relative contribution of each arsenic species. To address this data gap, the authors conducted an in-depth review of available information on speciated arsenic in air. The evaluation included the type of species measured and the relative abundance, as well as an analysis of the limitations of current analytical methods. Despite inherent differences in the procedures, most techniques effectively separated arsenic species in the air samples. Common analytical techniques such as inductively coupled plasma mass spectrometry (ICP-MS) and/or hydride generation (HG)- or quartz furnace (GF)-atomic absorption spectrometry (AAS) were used for arsenic measurement in the extracts, and provided some of the most sensitive detection limits. The current analysis demonstrated that, despite limited comparability among studies due to differences in seasonal factors, study duration, sample collection methods, and analytical methods, research conducted to date is adequate to show that arsenic in air is mainly in the inorganic form. Reported average concentrations of As(III) and As(V) ranged up to 7.4 and 10.4 ng/m3, respectively, with As(V) being more prevalent than As(III) in most studies. Concentrations of the organic methylated arsenic compounds are negligible (in the pg/m3 range). However because of the variability in study methods and measurement methodology, the authors were unable to determine the variation in arsenic composition as a function of source or particulate matter (PM) fraction. In this work, the authors include the implications of arsenic speciation in air on potential exposure and risks. The authors conclude that it is important to synchronize sample collection, preparation, and analytical techniques in order to generate

Double-contained receiver tank 244-TX, grab samples, 244TX-97-1 through 244TX-97-3 analytical results for the final report

International Nuclear Information System (INIS)

Esch, R.A.

1997-01-01

This document is the final report for the double-contained receiver tank (DCRT) 244-TX grab samples. Three grabs samples were collected from riser 8 on May 29, 1997. Analyses were performed in accordance with the Compatibility Grab Sampling and Analysis Plan (TSAP) and the Data Quality Objectives for Tank Farms Waste Compatibility Program (DQO). The analytical results are presented in a table

A Systematic Review of Published Respondent-Driven Sampling Surveys Collecting Behavioral and Biologic Data.

Science.gov (United States)

Johnston, Lisa G; Hakim, Avi J; Dittrich, Samantha; Burnett, Janet; Kim, Evelyn; White, Richard G

2016-08-01

Reporting key details of respondent-driven sampling (RDS) survey implementation and analysis is essential for assessing the quality of RDS surveys. RDS is both a recruitment and analytic method and, as such, it is important to adequately describe both aspects in publications. We extracted data from peer-reviewed literature published through September, 2013 that reported collected biological specimens using RDS. We identified 151 eligible peer-reviewed articles describing 222 surveys conducted in seven regions throughout the world. Most published surveys reported basic implementation information such as survey city, country, year, population sampled, interview method, and final sample size. However, many surveys did not report essential methodological and analytical information for assessing RDS survey quality, including number of recruitment sites, seeds at start and end, maximum number of waves, and whether data were adjusted for network size. Understanding the quality of data collection and analysis in RDS is useful for effectively planning public health service delivery and funding priorities.

Recent analytical applications of magnetic nanoparticles

Directory of Open Access Journals (Sweden)

Mohammad Faraji

2016-07-01

Full Text Available Analytical chemistry has experienced, as well as other areas of science, a big change due to the needs and opportunities provided by analytical nanoscience and nanotechnology. Now, nanotechnology is increasingly proving to be a powerful ally of analytical chemistry to achieve its objectives, and to simplify analytical processes. Moreover, the information needs arising from the growing nanotechnological activity are opening an exciting new field of action for analytical chemists. Magnetic nanoparticles have been used in various fields owing to their unique properties including large specific surface area and simple separation with magnetic fields. For Analytical applications, they have been used mainly for sample preparation techniques (magnetic solid phase extraction with different advanced functional groups (layered double hydroxide, β-cyclodextrin, carbon nanotube, graphen, polymer, octadecylsilane and automation of it, microextraction techniques enantioseparation and chemosensors. This review summarizes the basic principles and achievements of magnetic nanoparticles in sample preparation techniques, enantioseparation and chemosensors. Also, some selected articles recently published (2010-2016 have been reviewed and discussed.

New classification of natural breeding habitats for Neotropical anophelines in the Yanomami Indian Reserve, Amazon Region, Brazil and a new larval sampling methodology.

Science.gov (United States)

Sánchez-Ribas, Jordi; Oliveira-Ferreira, Joseli; Rosa-Freitas, Maria Goreti; Trilla, Lluís; Silva-do-Nascimento, Teresa Fernandes

2015-09-01

Here we present the first in a series of articles about the ecology of immature stages of anophelines in the Brazilian Yanomami area. We propose a new larval habitat classification and a new larval sampling methodology. We also report some preliminary results illustrating the applicability of the methodology based on data collected in the Brazilian Amazon rainforest in a longitudinal study of two remote Yanomami communities, Parafuri and Toototobi. In these areas, we mapped and classified 112 natural breeding habitats located in low-order river systems based on their association with river flood pulses, seasonality and exposure to sun. Our classification rendered seven types of larval habitats: lakes associated with the river, which are subdivided into oxbow lakes and nonoxbow lakes, flooded areas associated with the river, flooded areas not associated with the river, rainfall pools, small forest streams, medium forest streams and rivers. The methodology for larval sampling was based on the accurate quantification of the effective breeding area, taking into account the area of the perimeter and subtypes of microenvironments present per larval habitat type using a laser range finder and a small portable inflatable boat. The new classification and new sampling methodology proposed herein may be useful in vector control programs.

New classification of natural breeding habitats for Neotropical anophelines in the Yanomami Indian Reserve, Amazon Region, Brazil and a new larval sampling methodology

Directory of Open Access Journals (Sweden)

Jordi Sánchez-Ribas

2015-09-01

Full Text Available Here we present the first in a series of articles about the ecology of immature stages of anophelines in the Brazilian Yanomami area. We propose a new larval habitat classification and a new larval sampling methodology. We also report some preliminary results illustrating the applicability of the methodology based on data collected in the Brazilian Amazon rainforest in a longitudinal study of two remote Yanomami communities, Parafuri and Toototobi. In these areas, we mapped and classified 112 natural breeding habitats located in low-order river systems based on their association with river flood pulses, seasonality and exposure to sun. Our classification rendered seven types of larval habitats: lakes associated with the river, which are subdivided into oxbow lakes and nonoxbow lakes, flooded areas associated with the river, flooded areas not associated with the river, rainfall pools, small forest streams, medium forest streams and rivers. The methodology for larval sampling was based on the accurate quantification of the effective breeding area, taking into account the area of the perimeter and subtypes of microenvironments present per larval habitat type using a laser range finder and a small portable inflatable boat. The new classification and new sampling methodology proposed herein may be useful in vector control programs.

Analytical challenges in sports drug testing.

Science.gov (United States)

Thevis, Mario; Krug, Oliver; Geyer, Hans; Walpurgis, Katja; Baume, Norbert; Thomas, Andreas

2018-03-01

Analytical chemistry represents a central aspect of doping controls. Routine sports drug testing approaches are primarily designed to address the question whether a prohibited substance is present in a doping control sample and whether prohibited methods (for example, blood transfusion or sample manipulation) have been conducted by an athlete. As some athletes have availed themselves of the substantial breadth of research and development in the pharmaceutical arena, proactive and preventive measures are required such as the early implementation of new drug candidates and corresponding metabolites into routine doping control assays, even though these drug candidates are to date not approved for human use. Beyond this, analytical data are also cornerstones of investigations into atypical or adverse analytical findings, where the overall picture provides ample reason for follow-up studies. Such studies have been of most diverse nature, and tailored approaches have been required to probe hypotheses and scenarios reported by the involved parties concerning the plausibility and consistency of statements and (analytical) facts. In order to outline the variety of challenges that doping control laboratories are facing besides providing optimal detection capabilities and analytical comprehensiveness, selected case vignettes involving the follow-up of unconventional adverse analytical findings, urine sample manipulation, drug/food contamination issues, and unexpected biotransformation reactions are thematized.

Go-flow: a reliability analysis methodology applicable to piping system

International Nuclear Information System (INIS)

Matsuoka, T.; Kobayashi, M.

1985-01-01

Since the completion of the Reactor Safety Study, the use of probabilistic risk assessment technique has been becoming more widespread in the nuclear community. Several analytical methods are used for the reliability analysis of nuclear power plants. The GO methodology is one of these methods. Using the GO methodology, the authors performed a reliability analysis of the emergency decay heat removal system of the nuclear ship Mutsu, in order to examine its applicability to piping systems. By this analysis, the authors have found out some disadvantages of the GO methodology. In the GO methodology, the signal is on-to-off or off-to-on signal, therefore the GO finds out the time point at which the state of a system changes, and can not treat a system which state changes as off-on-off. Several computer runs are required to obtain the time dependent failure probability of a system. In order to overcome these disadvantages, the authors propose a new analytical methodology: GO-FLOW. In GO-FLOW, the modeling method (chart) and the calculation procedure are similar to those in the GO methodology, but the meaning of signal and time point, and the definitions of operators are essentially different. In the paper, the GO-FLOW methodology is explained and two examples of the analysis by GO-FLOW are given

Analytical Chemistry Laboratory (ACL) procedure compendium. Volume 1, Administrative

Energy Technology Data Exchange (ETDEWEB)

1992-06-01

Covered are: analytical laboratory operations (ALO) sample receipt and control, ALO data report/package preparation review and control, single shell tank (PST) project sample tracking system, sample receiving, analytical balances, duties and responsibilities of sample custodian, sample refrigerator temperature monitoring, security, assignment of staff responsibilities, sample storage, data reporting, and general requirements for glassware.

A new analytical application of nylon-induced room-temperature phosphorescence: Determination of thiabendazole in water samples

Energy Technology Data Exchange (ETDEWEB)

Correa, R.A. [Departamento de Quimica Analitica, Facultad de Ciencias Bioquimicas y Farmaceuticas, Universidad Nacional de Rosario, Suipacha 531 (2000) Rosario (Argentina); Escandar, G.M. [Departamento de Quimica Analitica, Facultad de Ciencias Bioquimicas y Farmaceuticas, Universidad Nacional de Rosario, Suipacha 531 (2000) Rosario (Argentina)]. E-mail: gescanda@fbioyf.unr.edu.ar

2006-06-30

This paper discusses the first analytical determination of the widely used fungicide thiabendazole by nylon-induced phosphorimetry. Nylon was investigated as a novel solid-matrix for inducing room-temperature phosphorescence of thiabendazole, which was enhanced under the effect of external heavy-atom salts. Among the investigated salts, lead(II) acetate was the most effective in yielding a high phosphorescence signal. An additional enhancement of the phosphorescence emission was attained when the measurements were carried out under a nitrogen atmosphere. There was only a moderate increase in the presence of cyclodextrins. The room-temperature phosphorescence lifetimes of the adsorbed thiabendazole were measured under different working conditions and, in all cases, two decaying components were detected. On the basis of the obtained results, a very simple and sensitive phosphorimetric method for the determination of thiabendazole was established. The analytical figures of merit obtained under the best experimental conditions were: linear calibration range from 0.031 to 0.26 {mu}g ml{sup -1} (the lowest value corresponds to the quantitation limit), relative standard deviation, 2.4% (n = 5) at a level of 0.096 {mu}g ml{sup -1}, and limit of detection calculated according to 1995 IUPAC Recommendations equal to 0.010 {mu}g ml{sup -1} (0.03 ng/spot). The potential interference from common agrochemicals was also studied. The feasibility of determining thiabendazole in real samples was successfully evaluated through the analysis of spiked river, tap and mineral water samples.

Transuranic waste characterization sampling and analysis methods manual. Revision 1

International Nuclear Information System (INIS)

Suermann, J.F.

1996-04-01

This Methods Manual provides a unified source of information on the sampling and analytical techniques that enable Department of Energy (DOE) facilities to comply with the requirements established in the current revision of the Transuranic Waste Characterization Quality Assurance Program Plan (QAPP) for the Waste Isolation Pilot Plant (WIPP) Transuranic (TRU) Waste Characterization Program (the Program) and the WIPP Waste Analysis Plan. This Methods Manual includes all of the testing, sampling, and analytical methodologies accepted by DOE for use in implementing the Program requirements specified in the QAPP and the WIPP Waste Analysis Plan. The procedures in this Methods Manual are comprehensive and detailed and are designed to provide the necessary guidance for the preparation of site-specific procedures. With some analytical methods, such as Gas Chromatography/Mass Spectrometry, the Methods Manual procedures may be used directly. With other methods, such as nondestructive characterization, the Methods Manual provides guidance rather than a step-by-step procedure. Sites must meet all of the specified quality control requirements of the applicable procedure. Each DOE site must document the details of the procedures it will use and demonstrate the efficacy of such procedures to the Manager, National TRU Program Waste Characterization, during Waste Characterization and Certification audits

A procedure for the determination of Po-210 in water samples by alpha spectrometry

International Nuclear Information System (INIS)

2009-01-01

Reliable, comparable and 'fit for purpose' results are an essential requirement for any decision based on analytical measurements. For the analyst, the availability of tested and validated analytical procedures is a extremely important tool for production of such analytical measurements. For maximum utility, such procedures should be comprehensive, clearly formulated, and readily available to both the analyst and the customer for reference. Since 2004 the Environment programme of the IAEA has included activities aimed at the development of a set of procedures for the determination of radionuclides in terrestrial environmental samples. In the case of 210 Po, this started with the collection and review of about 130 papers from the scientific literature. Based on this review, two candidate methods for the chemical separation of 210 Po from water samples were selected for testing, refinement and validation in accordance with ISO guidelines. A comprehensive methodology for calculation of results including quantification of measurement uncertainty was also developed. This report presents the final procedure which was developed based on that work

Efficiency of analytical and sampling-based uncertainty propagation in intensity-modulated proton therapy

Science.gov (United States)

Wahl, N.; Hennig, P.; Wieser, H. P.; Bangert, M.

2017-07-01

The sensitivity of intensity-modulated proton therapy (IMPT) treatment plans to uncertainties can be quantified and mitigated with robust/min-max and stochastic/probabilistic treatment analysis and optimization techniques. Those methods usually rely on sparse random, importance, or worst-case sampling. Inevitably, this imposes a trade-off between computational speed and accuracy of the uncertainty propagation. Here, we investigate analytical probabilistic modeling (APM) as an alternative for uncertainty propagation and minimization in IMPT that does not rely on scenario sampling. APM propagates probability distributions over range and setup uncertainties via a Gaussian pencil-beam approximation into moments of the probability distributions over the resulting dose in closed form. It supports arbitrary correlation models and allows for efficient incorporation of fractionation effects regarding random and systematic errors. We evaluate the trade-off between run-time and accuracy of APM uncertainty computations on three patient datasets. Results are compared against reference computations facilitating importance and random sampling. Two approximation techniques to accelerate uncertainty propagation and minimization based on probabilistic treatment plan optimization are presented. Runtimes are measured on CPU and GPU platforms, dosimetric accuracy is quantified in comparison to a sampling-based benchmark (5000 random samples). APM accurately propagates range and setup uncertainties into dose uncertainties at competitive run-times (GPU ≤slant {5} min). The resulting standard deviation (expectation value) of dose show average global γ{3% / {3}~mm} pass rates between 94.2% and 99.9% (98.4% and 100.0%). All investigated importance sampling strategies provided less accuracy at higher run-times considering only a single fraction. Considering fractionation, APM uncertainty propagation and treatment plan optimization was proven to be possible at constant time complexity

APPLICATION OF LOT QUALITY ASSURANCE SAMPLING FOR ASSESSING DISEASE CONTROL PROGRAMMES - EXAMINATION OF SOME METHODOLOGICAL ISSUES

OpenAIRE

T. R. RAMESH RAO

2011-01-01

Lot Quality Assurance Sampling (LQAS), a statistical tool in industrial setup, has been in use since 1980 for monitoring and evaluation of programs on disease control / immunization status among children / health workers performance in health system. While conducting LQAS in the field, there are occasions, even after due care of design, there are practical and methodological issues to be addressed before it is recommended for implementation and intervention. LQAS is applied under the assumpti...

Supercritical Fluid Extraction and Ultra Performance Liquid Chromatography of Respiratory Quinones for Microbial Community Analysis in Environmental and Biological Samples

Directory of Open Access Journals (Sweden)

Koichi Fujie

2012-03-01

Full Text Available Microbial community structure plays a significant role in environmental assessment and animal health management. The development of a superior analytical strategy for the characterization of microbial community structure is an ongoing challenge. In this study, we developed an effective supercritical fluid extraction (SFE and ultra performance liquid chromatography (UPLC method for the analysis of bacterial respiratory quinones (RQ in environmental and biological samples. RQ profile analysis is one of the most widely used culture-independent tools for characterizing microbial community structure. A UPLC equipped with a photo diode array (PDA detector was successfully applied to the simultaneous determination of ubiquinones (UQ and menaquinones (MK without tedious pretreatment. Supercritical carbon dioxide (scCO2 extraction with the solid-phase cartridge trap proved to be a more effective and rapid method for extracting respiratory quinones, compared to a conventional organic solvent extraction method. This methodology leads to a successful analytical procedure that involves a significant reduction in the complexity and sample preparation time. Application of the optimized methodology to characterize microbial communities based on the RQ profile was demonstrated for a variety of environmental samples (activated sludge, digested sludge, and compost and biological samples (swine and Japanese quail feces.

Chemical analysis of geological samples

International Nuclear Information System (INIS)

Malhotra, R.K.

1997-01-01

Most of the analytical methodology used in geochemical exploration has been based on molecular absorption, atomic absorption, and ICP-AES, ICPMAS etc. Detection limit and precision are factors in the choice of methodology in search of metallic ores and are related to the accuracy of data. A brief outline of the various chemical analysis techniques explaining essentially the basics of measurement principles and instrumentation is discussed

Analytical Model of the Nonlinear Dynamics of Cantilever Tip-Sample Surface Interactions for Various Acoustic-Atomic Force Microscopies

Science.gov (United States)

Cantrell, John H., Jr.; Cantrell, Sean A.

2008-01-01

A comprehensive analytical model of the interaction of the cantilever tip of the atomic force microscope (AFM) with the sample surface is developed that accounts for the nonlinearity of the tip-surface interaction force. The interaction is modeled as a nonlinear spring coupled at opposite ends to linear springs representing cantilever and sample surface oscillators. The model leads to a pair of coupled nonlinear differential equations that are solved analytically using a standard iteration procedure. Solutions are obtained for the phase and amplitude signals generated by various acoustic-atomic force microscope (A-AFM) techniques including force modulation microscopy, atomic force acoustic microscopy, ultrasonic force microscopy, heterodyne force microscopy, resonant difference-frequency atomic force ultrasonic microscopy (RDF-AFUM), and the commonly used intermittent contact mode (TappingMode) generally available on AFMs. The solutions are used to obtain a quantitative measure of image contrast resulting from variations in the Young modulus of the sample for the amplitude and phase images generated by the A-AFM techniques. Application of the model to RDF-AFUM and intermittent soft contact phase images of LaRC-cp2 polyimide polymer is discussed. The model predicts variations in the Young modulus of the material of 24 percent from the RDF-AFUM image and 18 percent from the intermittent soft contact image. Both predictions are in good agreement with the literature value of 21 percent obtained from independent, macroscopic measurements of sheet polymer material.

EnergiTools. A methodology for performance monitoring and diagnosis

International Nuclear Information System (INIS)

Ancion, P.; Bastien, R.; Ringdahl, K.

2000-01-01

EnergiTools is a performance monitoring and diagnostic tool that combines the power of on-line process data acquisition with advanced diagnosis methodologies. Analytical models based on thermodynamic principles are combined with neural networks to validate sensor data and to estimate missing or faulty measurements. Advanced diagnostic technologies are then applied to point out potential faults and areas to be investigated further. The diagnosis methodologies are based on Bayesian belief networks. Expert knowledge is captured in the form of the fault-symptom relationships and includes historical information as the likelihood of faults and symptoms. The methodology produces the likelihood of component failure root causes using the expert knowledge base. EnergiTools is used at Ringhals nuclear power plants. It has led to the diagnosis of various performance issues. Three case studies based on this plant data and model are presented and illustrate the diagnosis support methodologies implemented in EnergiTools . In the first case, the analytical data qualification technique points out several faulty measurements. The application of a neural network for the estimation of the nuclear reactor power by interpreting several plant indicators is then illustrated. The use of the Bayesian belief networks is finally described. (author)

Rapid and Automated Determination of Plutonium and Neptunium in Environmental Samples

DEFF Research Database (Denmark)

Qiao, Jixin

This thesis presents improved analytical methods for rapid and automated determination of plutonium and neptunium in environmental samples using sequential injection (SI) based chromatography and inductively coupled plasma mass spectrometry (ICP-MS). The progress of methodology development...... and optimization for rapid determination of plutonium in environmental samples using SIextraction chromatography prior to inductively coupled plasma mass spectrometry (Paper III); (3) Development of an SI-chromatographic method for simultaneous determination of plutonium and neptunium in environmental samples...... for rapid and simultaneous determination of plutonium and neptunium within an SI system (Paper VI). The results demonstrate that the developed methods in this study are reliable and efficient for accurate assays of trace levels of plutonium and neptunium as demanded in different situations including...

Procedure for hazards analysis of plutonium gloveboxes used in analytical chemistry operations

International Nuclear Information System (INIS)

Delvin, W.L.

1977-06-01

A procedure is presented to identify and assess hazards associated with gloveboxes used for analytical chemistry operations involving plutonium. This procedure is based upon analytic tree methodology and it has been adapted from the US Energy Research and Development Administration's safety program, the Management Oversight and Risk Tree

[Pre-analytical stability before centrifugation of 7 biochemical analytes in whole blood].

Science.gov (United States)

Perrier-Cornet, Andreas; Moineau, Marie-Pierre; Narbonne, Valérie; Plee-Gautier, Emmanuelle; Le Saos, Fabienne; Carre, Jean-Luc

2015-01-01

The pre-analytical stability of 7 biochemical parameters (parathyroid hormone -PTH-, vitamins A, C E and D, 1,25-dihydroxyvitamin D and insulin) at +4 °C, was studied on whole blood samples before centrifugation. The impact of freezing at -20°C was also analyzed/performed for PTH and vitamin D. The differences in the results of assays for whole blood samples, being kept for different times between sampling time and analysis, from 9 healthy adults, were compaired by using a Student t test. The 7 analytes investigated remained stable up to 4 hours at +4°C in whole blood. This study showed that it is possible to accept uncentrifuged whole blood specimens kept at +4°C before analysis. PTH is affected by freezing whereas vitamin D is not.

Lean six sigma methodologies improve clinical laboratory efficiency and reduce turnaround times.

Science.gov (United States)

Inal, Tamer C; Goruroglu Ozturk, Ozlem; Kibar, Filiz; Cetiner, Salih; Matyar, Selcuk; Daglioglu, Gulcin; Yaman, Akgun

2018-01-01

Organizing work flow is a major task of laboratory management. Recently, clinical laboratories have started to adopt methodologies such as Lean Six Sigma and some successful implementations have been reported. This study used Lean Six Sigma to simplify the laboratory work process and decrease the turnaround time by eliminating non-value-adding steps. The five-stage Six Sigma system known as define, measure, analyze, improve, and control (DMAIC) is used to identify and solve problems. The laboratory turnaround time for individual tests, total delay time in the sample reception area, and percentage of steps involving risks of medical errors and biological hazards in the overall process are measured. The pre-analytical process in the reception area was improved by eliminating 3 h and 22.5 min of non-value-adding work. Turnaround time also improved for stat samples from 68 to 59 min after applying Lean. Steps prone to medical errors and posing potential biological hazards to receptionists were reduced from 30% to 3%. Successful implementation of Lean Six Sigma significantly improved all of the selected performance metrics. This quality-improvement methodology has the potential to significantly improve clinical laboratories. © 2017 Wiley Periodicals, Inc.

Nationwide Multicenter Reference Interval Study for 28 Common Biochemical Analytes in China.

Science.gov (United States)

Xia, Liangyu; Chen, Ming; Liu, Min; Tao, Zhihua; Li, Shijun; Wang, Liang; Cheng, Xinqi; Qin, Xuzhen; Han, Jianhua; Li, Pengchang; Hou, Li'an; Yu, Songlin; Ichihara, Kiyoshi; Qiu, Ling

2016-03-01

A nationwide multicenter study was conducted in the China to explore sources of variation of reference values and establish reference intervals for 28 common biochemical analytes, as a part of the International Federation of Clinical Chemistry and Laboratory Medicine, Committee on Reference Intervals and Decision Limits (IFCC/C-RIDL) global study on reference values. A total of 3148 apparently healthy volunteers were recruited in 6 cities covering a wide area in China. Blood samples were tested in 2 central laboratories using Beckman Coulter AU5800 chemistry analyzers. Certified reference materials and value-assigned serum panel were used for standardization of test results. Multiple regression analysis was performed to explore sources of variation. Need for partition of reference intervals was evaluated based on 3-level nested ANOVA. After secondary exclusion using the latent abnormal values exclusion method, reference intervals were derived by a parametric method using the modified Box-Cox formula. Test results of 20 analytes were made traceable to reference measurement procedures. By the ANOVA, significant sex-related and age-related differences were observed in 12 and 12 analytes, respectively. A small regional difference was observed in the results for albumin, glucose, and sodium. Multiple regression analysis revealed BMI-related changes in results of 9 analytes for man and 6 for woman. Reference intervals of 28 analytes were computed with 17 analytes partitioned by sex and/or age. In conclusion, reference intervals of 28 common chemistry analytes applicable to Chinese Han population were established by use of the latest methodology. Reference intervals of 20 analytes traceable to reference measurement procedures can be used as common reference intervals, whereas others can be used as the assay system-specific reference intervals in China.

Electrophoretic extraction of low molecular weight cationic analytes from sodium dodecyl sulfate containing sample matrices for their direct electrospray ionization mass spectrometry.

Science.gov (United States)

Kinde, Tristan F; Lopez, Thomas D; Dutta, Debashis

2015-03-03

While the use of sodium dodecyl sulfate (SDS) in separation buffers allows efficient analysis of complex mixtures, its presence in the sample matrix is known to severely interfere with the mass-spectrometric characterization of analyte molecules. In this article, we report a microfluidic device that addresses this analytical challenge by enabling inline electrospray ionization mass spectrometry (ESI-MS) of low molecular weight cationic samples prepared in SDS containing matrices. The functionality of this device relies on the continuous extraction of analyte molecules into an SDS-free solvent stream based on the free-flow zone electrophoresis (FFZE) technique prior to their ESI-MS analysis. The reported extraction was accomplished in our current work in a glass channel with microelectrodes fabricated along its sidewalls to realize the desired electric field. Our experiments show that a key challenge to successfully operating such a device is to suppress the electroosmotically driven fluid circulations generated in its extraction channel that otherwise tend to vigorously mix the liquid streams flowing through this duct. A new coating medium, N-(2-triethoxysilylpropyl) formamide, recently demonstrated by our laboratory to nearly eliminate electroosmotic flow in glass microchannels was employed to address this issue. Applying this surface modifier, we were able to efficiently extract two different peptides, human angiotensin I and MRFA, individually from an SDS containing matrix using the FFZE method and detect them at concentrations down to 3.7 and 6.3 μg/mL, respectively, in samples containing as much as 10 mM SDS. Notice that in addition to greatly reducing the amount of SDS entering the MS instrument, the reported approach allows rapid solvent exchange for facilitating efficient analyte ionization desired in ESI-MS analysis.

Pre-analytical and analytical validations and clinical applications of a miniaturized, simple and cost-effective solid phase extraction combined with LC-MS/MS for the simultaneous determination of catecholamines and metanephrines in spot urine samples.

Science.gov (United States)

Li, Xiaoguang Sunny; Li, Shu; Kellermann, Gottfried

2016-10-01

It remains a challenge to simultaneously quantify catecholamines and metanephrines in a simple, sensitive and cost-effective manner due to pre-analytical and analytical constraints. Herein, we describe such a method consisting of a miniaturized sample preparation and selective LC-MS/MS detection by the use of second morning spot urine samples. Ten microliters of second morning urine sample were subjected to solid phase extraction on an Oasis HLB microplate upon complexation with phenylboronic acid. The analytes were well-resolved on a Luna PFP column followed by tandem mass spectrometric detection. Full validation and suitability of spot urine sampling and biological variation were investigated. The extraction recovery and matrix effect are 74.1-97.3% and 84.1-119.0%, respectively. The linearity range is 2.5-500, 0.5-500, 2.5-1250, 2.5-1250 and 0.5-1250ng/mL for norepinephrine, epinephrine, dopamine, normetanephrine and metanephrine, respectively. The intra- and inter-assay imprecisions are ≤9.4% for spiked quality control samples, and the respective recoveries are 97.2-112.5% and 95.9-104.0%. The Deming regression slope is 0.90-1.08, and the mean Bland-Altman percentage difference is from -3.29 to 11.85 between a published and proposed method (n=50). A correlation observed for the spot and 24h urine collections is significant (n=20, p<0.0001, r: 0.84-0.95, slope: 0.61-0.98). No statistical differences are found in day-to-day biological variability (n=20). Reference intervals are established for an apparently healthy population (n=88). The developed method, being practical, sensitive, reliable and cost-effective, is expected to set a new stage for routine testing, basic research and clinical applications. Copyright © 2016 Elsevier B.V. All rights reserved.

Irregular analytical errors in diagnostic testing - a novel concept.

Science.gov (United States)

Vogeser, Michael; Seger, Christoph

2018-02-23

In laboratory medicine, routine periodic analyses for internal and external quality control measurements interpreted by statistical methods are mandatory for batch clearance. Data analysis of these process-oriented measurements allows for insight into random analytical variation and systematic calibration bias over time. However, in such a setting, any individual sample is not under individual quality control. The quality control measurements act only at the batch level. Quantitative or qualitative data derived for many effects and interferences associated with an individual diagnostic sample can compromise any analyte. It is obvious that a process for a quality-control-sample-based approach of quality assurance is not sensitive to such errors. To address the potential causes and nature of such analytical interference in individual samples more systematically, we suggest the introduction of a new term called the irregular (individual) analytical error. Practically, this term can be applied in any analytical assay that is traceable to a reference measurement system. For an individual sample an irregular analytical error is defined as an inaccuracy (which is the deviation from a reference measurement procedure result) of a test result that is so high it cannot be explained by measurement uncertainty of the utilized routine assay operating within the accepted limitations of the associated process quality control measurements. The deviation can be defined as the linear combination of the process measurement uncertainty and the method bias for the reference measurement system. Such errors should be coined irregular analytical errors of the individual sample. The measurement result is compromised either by an irregular effect associated with the individual composition (matrix) of the sample or an individual single sample associated processing error in the analytical process. Currently, the availability of reference measurement procedures is still highly limited, but LC

Critical Discourse Analysis. The Elaboration of a Problem Oriented Discourse Analytic Approach After Foucault

Directory of Open Access Journals (Sweden)

Rainer Diaz-Bone

2006-05-01

Full Text Available Abstract: The German discourse researcher Siegfried JÄGER from Duisburg is the first to have published a German-language book about the methodology of discourse analysis after FOUCAULT. JÄGER integrates in his work the discourse analytic work of Jürgen LINK as well as the interdisciplinary discussion carried on in the discourse analytic journal "kultuRRevolution" (Journal for Applied Discourse Analysis. JÄGER and his co-workers were associated with the Duisburger Institute for Language Research and Social Research (DISS, see http://www.diss-duisburg.de/ for 20 years, developing discourse theory and the methodology of discourse analysis. The interview was done via e-mail. It depicts the discourse analytic approach of JÄGER and his co-workers following the works of FOUCAULT and LINK. The interview reconstructs JÄGERs vita and his academic career. Further topics of the interview are the agenda of JÄGERs discourse studies, methodological considerations, the (problematic relationship between FOUCAULDian discourse analysis and (discourses, linguistics, styles and organization of research and questions concerning applied discourse analytic research as a form of critical intervention. URN: urn:nbn:de:0114-fqs0603219

Sample preparation procedures utilized in microbial metabolomics: An overview.

Science.gov (United States)

Patejko, Małgorzata; Jacyna, Julia; Markuszewski, Michał J

2017-02-01

Bacteria are remarkably diverse in terms of their size, structure and biochemical properties. Due to this fact, it is hard to develop a universal method for handling bacteria cultures during metabolomic analysis. The choice of suitable processing methods constitutes a key element in any analysis, because only appropriate selection of procedures may provide accurate results, leading to reliable conclusions. Because of that, every analytical experiment concerning bacteria requires individually and very carefully planned research methodology. Although every study varies in terms of sample preparation, there are few general steps to follow while planning experiment, like sampling, separation of cells from growth medium, stopping their metabolism and extraction. As a result of extraction, all intracellular metabolites should be washed out from cell environment. What is more, extraction method utilized cannot cause any chemical decomposition or degradation of the metabolome. Furthermore, chosen extraction method should correlate with analytical technique, so it will not disturb or prolong following sample preparation steps. For those reasons, we observe a need to summarize sample preparation procedures currently utilized in microbial metabolomic studies. In the presented overview, papers concerning analysis of extra- and intracellular metabolites, published over the last decade, have been discussed. Presented work gives some basic guidelines that might be useful while planning experiments in microbial metabolomics. Copyright © 2016 Elsevier B.V. All rights reserved.

Quality assurance in the pre-analytical phase of human urine samples by (1)H NMR spectroscopy.

Science.gov (United States)

Budde, Kathrin; Gök, Ömer-Necmi; Pietzner, Maik; Meisinger, Christine; Leitzmann, Michael; Nauck, Matthias; Köttgen, Anna; Friedrich, Nele

2016-01-01

Metabolomic approaches investigate changes in metabolite profiles, which may reflect changes in metabolic pathways and provide information correlated with a specific biological process or pathophysiology. High-resolution (1)H NMR spectroscopy is used to identify metabolites in biofluids and tissue samples qualitatively and quantitatively. This pre-analytical study evaluated the effects of storage time and temperature on (1)H NMR spectra from human urine in two settings. Firstly, to evaluate short time effects probably due to acute delay in sample handling and secondly, the effect of prolonged storage up to one month to find markers of sample miss-handling. A number of statistical procedures were used to assess the differences between samples stored under different conditions, including Projection to Latent Structure Discriminant Analysis (PLS-DA), non-parametric testing as well as mixed effect linear regression analysis. The results indicate that human urine samples can be stored at 10 °C for 24 h or at -80 °C for 1 month, as no relevant changes in (1)H NMR fingerprints were observed during these time periods and temperature conditions. However, some metabolites most likely of microbial origin showed alterations during prolonged storage but without facilitating classification. In conclusion, the presented protocol for urine sample handling and semi-automatic metabolite quantification is suitable for large-scale epidemiological studies. Copyright © 2015 Elsevier Inc. All rights reserved.

Stability of Circulating Blood-Based MicroRNAs - Pre-Analytic Methodological Considerations

DEFF Research Database (Denmark)

Glinge, Charlotte; Clauss, Sebastian; Boddum, Kim

2017-01-01

BACKGROUND AND AIM: The potential of microRNAs (miRNA) as non-invasive diagnostic, prognostic, and predictive biomarkers, as well as therapeutic targets, has recently been recognized. Previous studies have highlighted the importance of consistency in the methodology used, but to our knowledge, no...

Evaluating Modeling Sessions Using the Analytic Hierarchy Process

NARCIS (Netherlands)

Ssebuggwawo, D.; Hoppenbrouwers, S.J.B.A.; Proper, H.A.; Persson, A.; Stirna, J.

2008-01-01

In this paper, which is methodological in nature, we propose to use an established method from the field of Operations Research, the Analytic Hierarchy Process (AHP), in the integrated, stakeholder- oriented evaluation of enterprise modeling sessions: their language, pro- cess, tool (medium), and

Forensic analysis of high explosives residues in post-blast water samples employing solid phase extraction for analyte pro-concentration

International Nuclear Information System (INIS)

Umi Kalsom Ahmad; Rajendran, Sumathy; Ling, Lee Woan

2008-01-01

Nitro aromatic, nitramine and nitrate ester compounds are a major group of high order explosive or better known as military explosives. Octahydro-1,3,5,7-tetrazocine (HMX), 1,3,5-hexahydro-1,3,5-trinitro triazine (RDX), 2,4,6-trinitro-toluene (TNT), pentaerythritol tetranitrate (PETN) and 2,4-dinitrotoluene (2,4-DNT) are secondary high explosives classified as most commonly used explosives components. There is an increasing demand for pre-concentration of these compounds in water samples as the sensitivity achieved by instrumental analytical methods for these high explosives residues are the main drawback in the application at trace levels for forensic analysis. Hence, a simple cartridge solid phase extraction (SPE) procedure was optimized as the off-line extraction and pre-concentration method to enhance the detection limit of high explosive residues using micellar electrokinetic chromatography (MEKC) and gas chromatography with electron-capture detection (GC-ECD) methods. The SPE cartridges utilized LiChrolut EN as the SPE adsorbent. By emplying pre-concentration using SPE, the detection limits of the target analytes in water sample were lowered by more than 1000 times with good percentage recovery (>87%) for MEKC method and lowered by 120 times with more than 2 % percentage recovery for GC-ECD methods. In order to test the feasibility of the developed method to real cases, post-blast water samples were analyzed. The post-blast water samples which were collected from Baling Bom training range, Ulu Kinta, Perak contained RDX and PETN in the range of 0.05 - 0.17 ppm and 0.0124 - 0.0390 ppm respectively. (author)

Quantifying construction and demolition waste: An analytical review

International Nuclear Information System (INIS)

Wu, Zezhou; Yu, Ann T.W.; Shen, Liyin; Liu, Guiwen

2014-01-01

Highlights: • Prevailing C and D waste quantification methodologies are identified and compared. • One specific methodology cannot fulfill all waste quantification scenarios. • A relevance tree for appropriate quantification methodology selection is proposed. • More attentions should be paid to civil and infrastructural works. • Classified information is suggested for making an effective waste management plan. - Abstract: Quantifying construction and demolition (C and D) waste generation is regarded as a prerequisite for the implementation of successful waste management. In literature, various methods have been employed to quantify the C and D waste generation at both regional and project levels. However, an integrated review that systemically describes and analyses all the existing methods has yet to be conducted. To bridge this research gap, an analytical review is conducted. Fifty-seven papers are retrieved based on a set of rigorous procedures. The characteristics of the selected papers are classified according to the following criteria - waste generation activity, estimation level and quantification methodology. Six categories of existing C and D waste quantification methodologies are identified, including site visit method, waste generation rate method, lifetime analysis method, classification system accumulation method, variables modelling method and other particular methods. A critical comparison of the identified methods is given according to their characteristics and implementation constraints. Moreover, a decision tree is proposed for aiding the selection of the most appropriate quantification method in different scenarios. Based on the analytical review, limitations of previous studies and recommendations of potential future research directions are further suggested

Critical evaluation of methodology commonly used in sample collection, storage and preparation for the analysis of pharmaceuticals and illicit drugs in surface water and wastewater by solid phase extraction and liquid chromatography-mass spectrometry.

Science.gov (United States)

Baker, David R; Kasprzyk-Hordern, Barbara

2011-11-04

The main aim of this manuscript is to provide a comprehensive and critical verification of methodology commonly used for sample collection, storage and preparation in studies concerning the analysis of pharmaceuticals and illicit drugs in aqueous environmental samples with the usage of SPE-LC/MS techniques. This manuscript reports the results of investigations into several sample preparation parameters that to the authors' knowledge have not been reported or have received very little attention. This includes: (i) effect of evaporation temperature and (ii) solvent with regards to solid phase extraction (SPE) extracts; (iii) effect of silanising glassware; (iv) recovery of analytes during vacuum filtration through glass fibre filters and (v) pre LC-MS filter membranes. All of these parameters are vital to develop efficient and reliable extraction techniques; an essential factor given that target drug residues are often present in the aqueous environment at ng L(-1) levels. Presented is also the first comprehensive review of the stability of illicit drugs and pharmaceuticals in wastewater. Among the parameters studied are: time of storage, temperature and pH. Over 60 analytes were targeted including stimulants, opioid and morphine derivatives, benzodiazepines, antidepressants, dissociative anaesthetics, drug precursors, human urine indicators and their metabolites. The lack of stability of analytes in raw wastewater was found to be significant for many compounds. For instance, 34% of compounds studied reported a stability change >15% after only 12 h in raw wastewater stored at 2 °C; a very important finding given that wastewater is typically collected with the use of 24 h composite samplers. The stability of these compounds is also critical given the recent development of so-called 'sewage forensics' or 'sewage epidemiology' in which concentrations of target drug residues in wastewater are used to back-calculate drug consumption. Without an understanding of stability

Liquid chromatography-tandem mass spectrometry analysis of perfluorooctane sulfonate and perfluorooctanoic Acid in fish fillet samples.

Science.gov (United States)

Paiano, Viviana; Fattore, Elena; Carrà, Andrea; Generoso, Caterina; Fanelli, Roberto; Bagnati, Renzo

2012-01-01

Perfluorooctane sulfonate (PFOS) and perfluorooctanoic (PFOA) acid are persistent contaminants which can be found in environmental and biological samples. A new and fast analytical method is described here for the analysis of these compounds in the edible part of fish samples. The method uses a simple liquid extraction by sonication, followed by a direct determination using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The linearity of the instrumental response was good, with average regression coefficients of 0.9971 and 0.9979 for PFOS and PFOA, respectively, and the coefficients of variation (CV) of the method ranged from 8% to 20%. Limits of detection (LOD) were 0.04 ng/g for both the analytes and recoveries were 90% for PFOS and 76% for PFOA. The method was applied to samples of homogenized fillets of wild and farmed fish from the Mediterranean Sea. Most of the samples showed little or no contamination by perfluorooctane sulfonate and perfluorooctanoic acid, and the highest concentrations detected among the fish species analyzed were, respectively, 5.96 ng/g and 1.89 ng/g. The developed analytical methodology can be used as a tool to monitor and to assess human exposure to perfluorinated compounds through sea food consumption.

Liquid Chromatography-Tandem Mass Spectrometry Analysis of Perfluorooctane Sulfonate and Perfluorooctanoic Acid in Fish Fillet Samples

Directory of Open Access Journals (Sweden)

Viviana Paiano

2012-01-01

Full Text Available Perfluorooctane sulfonate (PFOS and perfluorooctanoic (PFOA acid are persistent contaminants which can be found in environmental and biological samples. A new and fast analytical method is described here for the analysis of these compounds in the edible part of fish samples. The method uses a simple liquid extraction by sonication, followed by a direct determination using liquid chromatography-tandem mass spectrometry (LC-MS/MS. The linearity of the instrumental response was good, with average regression coefficients of 0.9971 and 0.9979 for PFOS and PFOA, respectively, and the coefficients of variation (CV of the method ranged from 8% to 20%. Limits of detection (LOD were 0.04 ng/g for both the analytes and recoveries were 90% for PFOS and 76% for PFOA. The method was applied to samples of homogenized fillets of wild and farmed fish from the Mediterranean Sea. Most of the samples showed little or no contamination by perfluorooctane sulfonate and perfluorooctanoic acid, and the highest concentrations detected among the fish species analyzed were, respectively, 5.96 ng/g and 1.89 ng/g. The developed analytical methodology can be used as a tool to monitor and to assess human exposure to perfluorinated compounds through sea food consumption.

Development of a fast capillary electrophoresis method for determination of carbohydrates in honey samples.

Science.gov (United States)

Rizelio, Viviane Maria; Tenfen, Laura; da Silveira, Roberta; Gonzaga, Luciano Valdemiro; Costa, Ana Carolina Oliveira; Fett, Roseane

2012-05-15

In this study, the determination of fructose, glucose and sucrose by capillary electrophoresis (CE) was investigated. The tendency of the analyte to undergo electromigration dispersion and the buffer capacity were evaluated using the Peakmaster(®) software and considered in the optimization of the background electrolyte, which was composed of 20 mmol L(-1) sorbic acid, 0.2 mmol L(-1) CTAB and 40 mmol L(-1) NaOH at pH 12.2. Under optimal CE conditions, the separation of the substances investigated was achieved in less than 2 min. The detection limits for the three analytes were in the range of 0.022 and 0.029 g L(-1) and precision measurements within 0.62-4.69% were achieved. The proposed methodology was applied in the quantitative analysis by direct injection of in honey samples to determine the main sugars presents. The samples were previously dissolved in deionized water and filtered with no other sample treatment. The mean values for fructose, glucose and sucrose were in the ranges of 33.65-45.46 g 100g(-1), 24.63-35.06 g 100g(-1) and <0.22-1.32 g 100g(-1), respectively. The good analytical performance of the method makes it suitable for implementation in food laboratories for the routine analysis of honey samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Risk methodology for geologic disposal of radioactive waste: interim report

International Nuclear Information System (INIS)

Campbell, J.E.; Dillon, R.T.; Tierney, M.S.; Davis, H.T.; McGrath, P.E.; Pearson, F.J. Jr.; Shaw, H.R.; Helton, J.C.; Donath, F.A.

1978-10-01

The Fuel Cycle Risk Analysis Division of Sandia Laboratories is funded by the Nuclear Regulatory Commission (NRC) to develop a methodology for assessment of the long-term risks from radioactive waste disposal in deep, geologic media. The first phase of this work, which is documented in this report, involves the following: (1) development of analytical models to represent the processes by which radioactive waste might leave the waste repository, enter the surface environment and eventually reach humans and (2) definition of a hypothetical ''reference system'' to provide a realistic setting for exercise of the models in a risk or safety assessment. The second phase of this work, which will be documented in a later report, will involve use of the analytical models in a demonstration risk or safety assessment of the reference system. The analytical methods and data developed in this study are expected to form the basis for a portion of the NRC repository licensing methodology

"On-off" switchable tool for food sample preparation: merging molecularly imprinting technology with stimuli-responsive blocks. Current status, challenges and highlighted applications.

Science.gov (United States)

Garcia, Raquel; Gomes da Silva, Marco D R; Cabrita, Maria João

2018-01-01

Sample preparation still remains a great challenge in the analytical workflow representing the most time-consuming and laborious step in analytical procedures. Ideally, sample pre-treatment procedures must be more selective, cheap, quick and environmental friendly. Molecular imprinting technology is a powerful tool in the development of highly selective sample preparation methodologies enabling to preconcentrate the analytes from a complex food matrix. Actually, the design and development of molecularly imprinted polymers-based functional materials that merge an enhancement of selectivity with a controllable and switchable mode of action by means of specific stimulus constitutes a hot research topic in the field of food analysis. Thus, combining the stimuli responsive mechanism and imprinting technology a new generation of materials are emerging. The application of these smart materials in sample preparation is in early stage of development, nevertheless new improvements will promote a new driven in the demanding field of food sample preparation. The new trends in the advancement of food sample preparation using these smart materials will be presented in this review and highlighted the most relevant applications in this particular area of knowledge. Copyright © 2017 Elsevier B.V. All rights reserved.

Governance Analytical Framework : an Approach to Health Systems ...

International Development Research Centre (IDRC) Digital Library (Canada)

Researchers will develop and test a methodology - Governance Analytical Framework - for analyzing and assessing the influence of governance pattern on health ... IDRC and the São Paulo Research Foundation (FAPESP) signed a scientific and technological cooperation agreement to support joint research projects in ...

Multicriteria decision analysis in ranking of analytical procedures for aldrin determination in water.

Science.gov (United States)

Tobiszewski, Marek; Orłowski, Aleksander

2015-03-27

The study presents the possibility of multi-criteria decision analysis (MCDA) application when choosing analytical procedures with low environmental impact. A type of MCDA, Preference Ranking Organization Method for Enrichment Evaluations (PROMETHEE), was chosen as versatile tool that meets all the analytical chemists--decision makers requirements. Twenty five analytical procedures for aldrin determination in water samples (as an example) were selected as input alternatives to MCDA analysis. Nine different criteria describing the alternatives were chosen from different groups--metrological, economical and the most importantly--environmental impact. The weights for each criterion were obtained from questionnaires that were sent to experts, giving three different scenarios for MCDA results. The results of analysis show that PROMETHEE is very promising tool to choose the analytical procedure with respect to its greenness. The rankings for all three scenarios placed solid phase microextraction and liquid phase microextraction--based procedures high, while liquid-liquid extraction, solid phase extraction and stir bar sorptive extraction--based procedures were placed low in the ranking. The results show that although some of the experts do not intentionally choose green analytical chemistry procedures, their MCDA choice is in accordance with green chemistry principles. The PROMETHEE ranking results were compared with more widely accepted green analytical chemistry tools--NEMI and Eco-Scale. As PROMETHEE involved more different factors than NEMI, the assessment results were only weakly correlated. Oppositely, the results of Eco-Scale assessment were well-correlated as both methodologies involved similar criteria of assessment. Copyright © 2015 Elsevier B.V. All rights reserved.

Glycoprotein Enrichment Analytical Techniques: Advantages and Disadvantages.

Science.gov (United States)

Zhu, R; Zacharias, L; Wooding, K M; Peng, W; Mechref, Y

2017-01-01

Protein glycosylation is one of the most important posttranslational modifications. Numerous biological functions are related to protein glycosylation. However, analytical challenges remain in the glycoprotein analysis. To overcome the challenges associated with glycoprotein analysis, many analytical techniques were developed in recent years. Enrichment methods were used to improve the sensitivity of detection, while HPLC and mass spectrometry methods were developed to facilitate the separation of glycopeptides/proteins and enhance detection, respectively. Fragmentation techniques applied in modern mass spectrometers allow the structural interpretation of glycopeptides/proteins, while automated software tools started replacing manual processing to improve the reliability and throughput of the analysis. In this chapter, the current methodologies of glycoprotein analysis were discussed. Multiple analytical techniques are compared, and advantages and disadvantages of each technique are highlighted. © 2017 Elsevier Inc. All rights reserved.

Microfluidic devices for sample clean-up and screening of biological samples

NARCIS (Netherlands)

Tetala, K.K.R.

2009-01-01

Analytical chemistry plays an important role in the separation and identification of analytes from raw samples (e.g. plant extracts, blood), but the whole analytical process is tedious, difficult to automate and time consuming. To overcome these drawbacks, the concept of μTAS (miniaturized total

High-throughput analysis using non-depletive SPME: challenges and applications to the determination of free and total concentrations in small sample volumes.

Science.gov (United States)

Boyacı, Ezel; Bojko, Barbara; Reyes-Garcés, Nathaly; Poole, Justen J; Gómez-Ríos, Germán Augusto; Teixeira, Alexandre; Nicol, Beate; Pawliszyn, Janusz

2018-01-18

In vitro high-throughput non-depletive quantitation of chemicals in biofluids is of growing interest in many areas. Some of the challenges facing researchers include the limited volume of biofluids, rapid and high-throughput sampling requirements, and the lack of reliable methods. Coupled to the above, growing interest in the monitoring of kinetics and dynamics of miniaturized biosystems has spurred the demand for development of novel and revolutionary methodologies for analysis of biofluids. The applicability of solid-phase microextraction (SPME) is investigated as a potential technology to fulfill the aforementioned requirements. As analytes with sufficient diversity in their physicochemical features, nicotine, N,N-Diethyl-meta-toluamide, and diclofenac were selected as test compounds for the study. The objective was to develop methodologies that would allow repeated non-depletive sampling from 96-well plates, using 100 µL of sample. Initially, thin film-SPME was investigated. Results revealed substantial depletion and consequent disruption in the system. Therefore, new ultra-thin coated fibers were developed. The applicability of this device to the described sampling scenario was tested by determining the protein binding of the analytes. Results showed good agreement with rapid equilibrium dialysis. The presented method allows high-throughput analysis using small volumes, enabling fast reliable free and total concentration determinations without disruption of system equilibrium.

Development and validation of analytical methodology for determination of polycyclic aromatic hydrocarbons (PAHS) in sediments. Assesment of Pedroso Park dam, Santo Andre, SP; Desenvolvimento e validacao de metodologia analitica para determinacao de hidrocarbonetos policiclicos aromaticos (HPAS) em sedimentos. Avaliacao da represa do Parque Pedroso, Santo Andre, SP

Energy Technology Data Exchange (ETDEWEB)

Brito, Carlos Fernando de

2009-07-01

The polycyclic aromatic hydrocarbons (PAHs), by being considered persistent contaminants, by their ubiquity in the environment and by the recognition of their genotoxicity, have stimulated research activities in order to determine and evaluate their sources, transport, processing, biological effects and accumulation in compartments of aquatic and terrestrial ecosystems. In this work, the matrix studied was sediment collected at Pedroso Park's dam at Santo Andre, SP. The analytical technique employed was liquid chromatography in reverse phase with a UV/Vis detector. Statistics treatment of the data was established during the process of developing the methodology for which there was reliable results. The steps involved were evaluated using the concept of Validation of Chemical Testing. The parameters selected for the analytical validation were selectivity, linearity, Working Range, Sensitivity, Accuracy, Precision, Limit of Detection, Limit of quantification and robustness. These parameters showed satisfactory results, allowing the application of the methodology, and is a simple method that allows the minimization of contamination and loss of compounds by over-handling. For the PAHs tested were no found positive results, above the limit of detection, in any of the samples collected in the first phase. But, at the second collection, were found small changes mainly acenaphthylene, fluorene and benzo[a]anthracene. Although the area is preserved, it is possible to realize little signs of contamination. (author)

Microchip-electrochemistry route for rapid screening of hydroquinone and arbutin from miscellaneous samples: Investigation of the robustness of a simple cross-injector system

International Nuclear Information System (INIS)

Crevillen, Agustin G.; Barrigas, Ines; Blasco, Antonio Javier; Gonzalez, Maria Cristina; Escarpa, Alberto

2006-01-01

This work examines in deep the analytical performance of an example of 'first-generation' microdevices: capillary electrophoresis microchip (CE) with end-channel electrochemical detection (ED). A hydroquinone and arbutin separation strategically chosen as route involving pharmaceutical-clinical testing, public safety and food control scenes was carried out. The reproducibility of the unpinched electrokinetic protocol was carefully studied and the technical possibility of working indiscriminately and/or sequentially with both simple cross-injectors was also demonstrated using a real sample (R.S.D.'s less than 7%). The robustness of the injection protocol allowed checking the state of the microchip/detector coupling and following the extraction efficiency of the analyte from real sample. Separation variables such as pH, ionic strength and, separation voltage were also carefully assayed and optimized. Analyte screening was performed using borate buffer (pH 9, 60 mM) in less than 180 s in the samples studied improving dramatically the analysis times used for the same analytes on a conventional scale (15 min), with good precision (R.S.D.'s ranging 5-10%), accuracy (recoveries ranging 90-110%) and acceptable resolution (Rs ≥ 1.0). In addition, the excellent analytical performance of the overall analytical method indicated the quality of the whole analytical microsystem and allowed to introduce the definition of robustness for methodologies developed into the 'lab-on-a-chip' scene

Microchip-electrochemistry route for rapid screening of hydroquinone and arbutin from miscellaneous samples: Investigation of the robustness of a simple cross-injector system

Energy Technology Data Exchange (ETDEWEB)

Crevillen, Agustin G. [Dpto. Quimica Analitica e Ingenieria Quimica, Universidad de Alcala, 28871 Alcala de Henares, Madrid (Spain); Barrigas, Ines [Dpto. Quimica Analitica e Ingenieria Quimica, Universidad de Alcala, 28871 Alcala de Henares, Madrid (Spain); Blasco, Antonio Javier [Dpto. Quimica Analitica e Ingenieria Quimica, Universidad de Alcala, 28871 Alcala de Henares, Madrid (Spain); Gonzalez, Maria Cristina [Dpto. Quimica Analitica e Ingenieria Quimica, Universidad de Alcala, 28871 Alcala de Henares, Madrid (Spain); Escarpa, Alberto [Dpto. Quimica Analitica e Ingenieria Quimica, Universidad de Alcala, 28871 Alcala de Henares, Madrid (Spain)]. E-mail: alberto.escarpa@uah.es

2006-03-15

This work examines in deep the analytical performance of an example of 'first-generation' microdevices: capillary electrophoresis microchip (CE) with end-channel electrochemical detection (ED). A hydroquinone and arbutin separation strategically chosen as route involving pharmaceutical-clinical testing, public safety and food control scenes was carried out. The reproducibility of the unpinched electrokinetic protocol was carefully studied and the technical possibility of working indiscriminately and/or sequentially with both simple cross-injectors was also demonstrated using a real sample (R.S.D.'s less than 7%). The robustness of the injection protocol allowed checking the state of the microchip/detector coupling and following the extraction efficiency of the analyte from real sample. Separation variables such as pH, ionic strength and, separation voltage were also carefully assayed and optimized. Analyte screening was performed using borate buffer (pH 9, 60 mM) in less than 180 s in the samples studied improving dramatically the analysis times used for the same analytes on a conventional scale (15 min), with good precision (R.S.D.'s ranging 5-10%), accuracy (recoveries ranging 90-110%) and acceptable resolution (Rs {>=} 1.0). In addition, the excellent analytical performance of the overall analytical method indicated the quality of the whole analytical microsystem and allowed to introduce the definition of robustness for methodologies developed into the 'lab-on-a-chip' scene.

An Analytic Hierarchy Process for School Quality and Inspection: Model Development and Application

Science.gov (United States)

Al Qubaisi, Amal; Badri, Masood; Mohaidat, Jihad; Al Dhaheri, Hamad; Yang, Guang; Al Rashedi, Asma; Greer, Kenneth

2016-01-01

Purpose: The purpose of this paper is to develop an analytic hierarchy planning-based framework to establish criteria weights and to develop a school performance system commonly called school inspections. Design/methodology/approach: The analytic hierarchy process (AHP) model uses pairwise comparisons and a measurement scale to generate the…

ISCO Grab Sample Ion Chromatography Analytical Data

Data.gov (United States)

U.S. Environmental Protection Agency — ISCO grab samples were collected from river, wastewater treatment plant discharge, and public drinking water intakes. Samples were analyzed for major ions (ppb)...

Contributions to sampling statistics

CERN Document Server

Conti, Pier; Ranalli, Maria

2014-01-01

This book contains a selection of the papers presented at the ITACOSM 2013 Conference, held in Milan in June 2013. ITACOSM is the bi-annual meeting of the Survey Sampling Group S2G of the Italian Statistical Society, intended as an international  forum of scientific discussion on the developments of theory and application of survey sampling methodologies and applications in human and natural sciences. The book gathers research papers carefully selected from both invited and contributed sessions of the conference. The whole book appears to be a relevant contribution to various key aspects of sampling methodology and techniques; it deals with some hot topics in sampling theory, such as calibration, quantile-regression and multiple frame surveys, and with innovative methodologies in important topics of both sampling theory and applications. Contributions cut across current sampling methodologies such as interval estimation for complex samples, randomized responses, bootstrap, weighting, modeling, imputati...

Double-Shell Tank (DST) Ventilation System Vapor Sampling and Analysis Plan

International Nuclear Information System (INIS)

SASAKI, L.M.

2000-01-01

This sampling and analysis plan (SAP) identifies characterization objectives pertaining to sample collection, laboratory analytical evaluation, and reporting requirements for vapor samples from the primary ventilation systems of the AN, AP, AW, and AY/AZ tank farms. Sampling will be performed in accordance with Data Quality Objectives for Regulatory Requirements for Hazardous and Radioactive Air Emissions Sampling and Analysis (Air DQO) (Mulkey 1999). The sampling will verify if current air emission estimates used in the permit application are correct and provide information for future air permit applications. Vapor samples will be obtained from tank farm ventilation systems, downstream from the tanks and upstream of any filtration. Samples taken in support of the DQO will consist of SUMMA(trademark) canisters, triple sorbent traps (TSTs), sorbent tube trains (STTs), polyurethane foam (PUF) samples. Particulate filter samples and tritium traps will be taken for radiation screening to allow the release of the samples for analysis. The following sections provide the general methodology and procedures to be used in the preparation, retrieval, transport, analysis, and reporting of results from the vapor samples

Simultaneous grouping and ranking with combination of SOM and TOPSIS for selection of preferable analytical procedure for furan determination in food.

Science.gov (United States)

Jędrkiewicz, Renata; Tsakovski, Stefan; Lavenu, Aurore; Namieśnik, Jacek; Tobiszewski, Marek

2018-02-01

Novel methodology for grouping and ranking with application of self-organizing maps and multicriteria decision analysis is presented. The dataset consists of 22 objects that are analytical procedures applied to furan determination in food samples. They are described by 10 variables, referred to their analytical performance, environmental and economic aspects. Multivariate statistics analysis allows to limit the amount of input data for ranking analysis. Assessment results show that the most beneficial procedures are based on microextraction techniques with GC-MS final determination. It is presented how the information obtained from both tools complement each other. The applicability of combination of grouping and ranking is also discussed. Copyright © 2017 Elsevier B.V. All rights reserved.

A clean laboratory for ultratrace analysis: the ultratrace analytical facility (UTAF)

International Nuclear Information System (INIS)

Jadhav, S.G.; Sounderajan, Suvarna; Kumar, Sanjukta A.; Udas, A.C.; Ramanathan, M.; Palrecha, M.M.; Sudersanan, M.

2003-06-01

Thare has been an increasing demand for the quantification of various elements at extremely low concentrations in a variety of samples such as high purity materials, environmental and biological samples. The need for a controlled environment to obtain reliable and reproducible data necessitates the use of strategies and practices to minimize contamination during the analytical procedure. This report describes the protocol observed in our clean laboratory to eliminate contamination and ensure low laboratory blanks and some of the methodologies developed to carry out the analysis. The analysis is carried out by Graphite Furnace Atomic Absorption Spectrometry and electrochemical techniques such as Anodic/ Cathodic / Adsorptive Stripping Voltammetry. Characterisation of 5N (total impurities 10 ppm) arsenic is routinely carried out. Al in serum of patients suffering from end stage renal failure are also analyzed. Pine leaves, spinach, carrot puree and milk powder have been characterized for Al and Hg content and bovine serum has been characterized for Cu, Zn, Na, K in samples as part of intercomparison exercises. (author)

What about N? A methodological study of sample-size reporting in focus group studies.

Science.gov (United States)

Carlsen, Benedicte; Glenton, Claire

2011-03-11

Focus group studies are increasingly published in health related journals, but we know little about how researchers use this method, particularly how they determine the number of focus groups to conduct. The methodological literature commonly advises researchers to follow principles of data saturation, although practical advise on how to do this is lacking. Our objectives were firstly, to describe the current status of sample size in focus group studies reported in health journals. Secondly, to assess whether and how researchers explain the number of focus groups they carry out. We searched PubMed for studies that had used focus groups and that had been published in open access journals during 2008, and extracted data on the number of focus groups and on any explanation authors gave for this number. We also did a qualitative assessment of the papers with regard to how number of groups was explained and discussed. We identified 220 papers published in 117 journals. In these papers insufficient reporting of sample sizes was common. The number of focus groups conducted varied greatly (mean 8.4, median 5, range 1 to 96). Thirty seven (17%) studies attempted to explain the number of groups. Six studies referred to rules of thumb in the literature, three stated that they were unable to organize more groups for practical reasons, while 28 studies stated that they had reached a point of saturation. Among those stating that they had reached a point of saturation, several appeared not to have followed principles from grounded theory where data collection and analysis is an iterative process until saturation is reached. Studies with high numbers of focus groups did not offer explanations for number of groups. Too much data as a study weakness was not an issue discussed in any of the reviewed papers. Based on these findings we suggest that journals adopt more stringent requirements for focus group method reporting. The often poor and inconsistent reporting seen in these

What about N? A methodological study of sample-size reporting in focus group studies

Directory of Open Access Journals (Sweden)

Glenton Claire

2011-03-01

Full Text Available Abstract Background Focus group studies are increasingly published in health related journals, but we know little about how researchers use this method, particularly how they determine the number of focus groups to conduct. The methodological literature commonly advises researchers to follow principles of data saturation, although practical advise on how to do this is lacking. Our objectives were firstly, to describe the current status of sample size in focus group studies reported in health journals. Secondly, to assess whether and how researchers explain the number of focus groups they carry out. Methods We searched PubMed for studies that had used focus groups and that had been published in open access journals during 2008, and extracted data on the number of focus groups and on any explanation authors gave for this number. We also did a qualitative assessment of the papers with regard to how number of groups was explained and discussed. Results We identified 220 papers published in 117 journals. In these papers insufficient reporting of sample sizes was common. The number of focus groups conducted varied greatly (mean 8.4, median 5, range 1 to 96. Thirty seven (17% studies attempted to explain the number of groups. Six studies referred to rules of thumb in the literature, three stated that they were unable to organize more groups for practical reasons, while 28 studies stated that they had reached a point of saturation. Among those stating that they had reached a point of saturation, several appeared not to have followed principles from grounded theory where data collection and analysis is an iterative process until saturation is reached. Studies with high numbers of focus groups did not offer explanations for number of groups. Too much data as a study weakness was not an issue discussed in any of the reviewed papers. Conclusions Based on these findings we suggest that journals adopt more stringent requirements for focus group method

Engendering Development: Some Methodological Perspectives on Child Labour

Directory of Open Access Journals (Sweden)

Erica Burman

2006-01-01

Full Text Available In this article I address when and why it is useful to focus on gender in the design and conceptualisation of developmental psychological research. Since methodological debates treated in the abstract tend to lack both the specificity and rigour that application to a particular context or topic imports, I take a particular focus for my discussion: child labour. In doing so I hope to highlight the analytical and practical gains of bringing gendered agendas alongside, and into, developmental research. While child labour may seem a rather curious topic for discussion of developmental psychological research practice, this article will show how it indicates with particular clarity issues that mainstream psychological research often occludes or forgets. In particular, I explore analytical and methodological benefits of exploring the diverse ways gender structures notions of childhood, alongside the developmental commonalities and asymmetries of gender and age as categories. I suggest that the usual assumed elision between women and children is often unhelpful for both women and children. Instead, an analytical attention to the shifting forms and relations of children's work facilitates more differentiated perspectives on how its meanings reflect economic and cultural (including gendered conditions, and so attends better to social inequalities. These inequalities also structure the methodological conditions and paradigms for research with children, and so the article finishes by elaborating from this discussion of child labour four key principles for engendering psychological research with and about children, which also have broader implications for conceptualisations of the relations between gender, childhood, culture and families. URN: urn:nbn:de:0114-fqs060111

A shipboard comparison of analytic methods for ballast water compliance monitoring

Science.gov (United States)

Bradie, Johanna; Broeg, Katja; Gianoli, Claudio; He, Jianjun; Heitmüller, Susanne; Curto, Alberto Lo; Nakata, Akiko; Rolke, Manfred; Schillak, Lothar; Stehouwer, Peter; Vanden Byllaardt, Julie; Veldhuis, Marcel; Welschmeyer, Nick; Younan, Lawrence; Zaake, André; Bailey, Sarah

2018-03-01

Promising approaches for indicative analysis of ballast water samples have been developed that require study in the field to examine their utility for determining compliance with the International Convention for the Control and Management of Ships' Ballast Water and Sediments. To address this gap, a voyage was undertaken on board the RV Meteor, sailing the North Atlantic Ocean from Mindelo (Cape Verde) to Hamburg (Germany) during June 4-15, 2015. Trials were conducted on local sea water taken up by the ship's ballast system at multiple locations along the trip, including open ocean, North Sea, and coastal water, to evaluate a number of analytic methods that measure the numeric concentration or biomass of viable organisms according to two size categories (≥ 50 μm in minimum dimension: 7 techniques, ≥ 10 μm and scientific approaches (e.g. flow cytometry). Several promising indicative methods were identified that showed high correlation with microscopy, but allow much quicker processing and require less expert knowledge. This study is the first to concurrently use a large number of analytic tools to examine a variety of ballast water samples on board an operational ship in the field. Results are useful to identify the merits of each method and can serve as a basis for further improvement and development of tools and methodologies for ballast water compliance monitoring.

Insights into PRA methodologies

International Nuclear Information System (INIS)

Gallagher, D.; Lofgren, E.; Atefi, B.; Liner, R.; Blond, R.; Amico, P.

1984-08-01

Probabilistic Risk Assessments (PRAs) for six nuclear power plants were examined to gain insight into how the choice of analytical methods can affect the results of PRAs. The PRA sreflectope considered was limited to internally initiated accidents sequences through core melt. For twenty methodological topic areas, a baseline or minimal methodology was specified. The choice of methods for each topic in the six PRAs was characterized in terms of the incremental level of effort above the baseline. A higher level of effort generally reflects a higher level of detail or a higher degree of sophistication in the analytical approach to a particular topic area. The impact on results was measured in terms of how additional effort beyond the baseline level changed the relative importance and ordering of dominant accident sequences compared to what would have been observed had methods corresponding to the baseline level of effort been employed. This measure of impact is a more useful indicator of how methods affect perceptions of plant vulnerabilities than changes in core melt frequency would be. However, the change in core melt frequency was used as a secondary measure of impact for nine topics where availability of information permitted. Results are presented primarily in the form of effort-impact matrices for each of the twenty topic areas. A suggested effort-impact profile for future PRAs is presented

Use of FTA® card methodology for sampling and molecular characterization of Echinococcus granulosus sensu lato in Africa.

Science.gov (United States)

Boué, Franck; El Berbri, Ikhlass; Hormaz, Vanessa; Boucher, Jean-Marc; El Mamy, Ahmed Bezeid; Traore, Abdallah; Fihri, Ouafaa Fassi; Petavy, Anne-Françoise; Dakkak, Allal; Umhang, Gérald

2017-02-01

Cystic Echinococcosis is a parasitic disease caused by the cestode Echinococcus granulosus widely distributed in Africa. Monitoring of this parasite requires access to cyst samples on intermediate hosts observed at the slaughterhouse. In order to facilitate sampling in the field and analysis, the French National Reference Laboratory for Echinococcus spp. has developed a tissue derived from DNA sampling with FTA ® card technology. The DNA samples were taken by applying the FTA ® paper on the germinal layer after opening the cysts. The sampling technique was validated using frozen cysts (n = 76) stored in the laboratory and from field samples (n = 134) taken at the slaughterhouse by veterinarian technicians during meat inspection in Morocco, Mali and Mauritania. DNA was extracted after several weeks of storage at room temperature. PCR assays were performed using primers for generic cestode (cox1) and amplified fragments were sequenced. All samples taken in the lab and 80% of field samples were capable of molecular characterization. Cyst-derived DNA from FTA ® samples can be useful for easy sampling, storage and rapid, safe and cheap shipment. The use of the FTA methodology will facilitate studies in the field to investigate the presence and genetic characterization of E. granulosus sensu lato in African countries. Copyright © 2016 Elsevier Inc. All rights reserved.

Analytical fingerprint for tantalum ores from African deposits

Science.gov (United States)

Melcher, F.; Graupner, T.; Sitnikova, M.; Oberthür, T.; Henjes-Kunst, F.; Gäbler, E.; Rantitsch, G.

2009-04-01

Illegal mining of gold, diamonds, copper, cobalt and, in the last decade, "coltan" has fuelled ongoing armed conflicts and civil war in a number of African countries. Following the United Nations initiative to fingerprint the origin of conflict materials and to develop a traceability system, our working group is investigating "coltan" (i.e. columbite-tantalite) mineralization especially in Africa, also within the wider framework of establishing certified trading chains (CTC). Special attention is directed towards samples from the main Ta-Nb-Sn provinces in Africa: DR Congo, Rwanda, Mozambique, Ethiopia, Egypt and Namibia. The following factors are taken into consideration in a methodological approach capable of distinguishing the origin of tantalum ores and concentrates with the utmost probability: (1) Quality and composition of coltan concentrates vary considerably. (2) Mineralogical and chemical compositions of Ta-Nb ores are extremely complex due to the wide range of the columbite-tantalite solid solution series and its ability to incorporate many additional elements. (3) Coltan concentrates may contain a number of other tantalum-bearing minerals besides columbite-tantalite. In our approach, coltan concentrates are analyzed in a step-by-step mode. State-of-the-art analytical tools employed are automated scanning electron microscopy (Mineral Liberation Analysis; MLA), electron microprobe analysis (major and trace elements), laser ablation-ICP-MS (trace elements, isotopes), and TIMS (U-Pb dating). Mineral assemblages in the ore concentrates, major and trace element concentration patterns, and zoning characteristics in the different pegmatites from Africa distinctly differ from each other. Chondrite-normalized REE distribution patterns vary significantly between columbite, tantalite, and microlite, and also relative to major element compositions of columbites. Some locations are characterized by low REE concentrations, others are highly enriched. Samples with

FACE Analysis as a Fast and Reliable Methodology to Monitor the Sulfation and Total Amount of Chondroitin Sulfate in Biological Samples of Clinical Importance

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Evgenia Karousou

2014-06-01

Full Text Available Glycosaminoglycans (GAGs due to their hydrophilic character and high anionic charge densities play important roles in various (pathophysiological processes. The identification and quantification of GAGs in biological samples and tissues could be useful prognostic and diagnostic tools in pathological conditions. Despite the noteworthy progress in the development of sensitive and accurate methodologies for the determination of GAGs, there is a significant lack in methodologies regarding sample preparation and reliable fast analysis methods enabling the simultaneous analysis of several biological samples. In this report, developed protocols for the isolation of GAGs in biological samples were applied to analyze various sulfated chondroitin sulfate- and hyaluronan-derived disaccharides using fluorophore-assisted carbohydrate electrophoresis (FACE. Applications to biologic samples of clinical importance include blood serum, lens capsule tissue and urine. The sample preparation protocol followed by FACE analysis allows quantification with an optimal linearity over the concentration range 1.0–220.0 µg/mL, affording a limit of quantitation of 50 ng of disaccharides. Validation of FACE results was performed by capillary electrophoresis and high performance liquid chromatography techniques.

Role of analytical chemistry in environmental monitoring

International Nuclear Information System (INIS)

Kayasth, S.; Swain, K.

2004-01-01

Basic aspects of pollution and the role of analytical chemistry in environmental monitoring are highlighted and exemplified, with emphasis on trace elements. Sources and pathways of natural and especially man-made polluting substances as well as physico-chemical characteristics are given. Attention is paid to adequate sampling in various compartments of the environment comprising both lithosphere and biosphere. Trace analysis is dealt with using a variety of analytical techniques, including criteria for choice of suited techniques, as well as aspects of analytical quality assurance and control. Finally, some data on trace elements levels in soil and water samples from India are presented. (author)

A Semi-Analytical Methodology for Multiwell Productivity Index of Well-Industry-Production-Scheme in Tight Oil Reservoirs

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Guangfeng Liu

2018-04-01

Full Text Available Recently, the well-industry-production-scheme (WIPS has attracted more and more attention to improve tight oil recovery. However, multi-well pressure interference (MWPI induced by well-industry-production-scheme (WIPS strongly challenges the traditional transient pressure analysis methods, which focus on single multi-fractured horizontal wells (SMFHWs without MWPI. Therefore, a semi-analytical methodology for multiwell productivity index (MPI was proposed to study well performance of WIPS scheme in tight reservoir. To facilitate methodology development, the conceptual models of tight formation and WIPS scheme were firstly described. Secondly, seepage models of tight reservoir and hydraulic fractures (HFs were sequentially established and then dynamically coupled. Numerical simulation was utilized to validate our model. Finally, identification of flow regimes and sensitivity analysis were conducted. Our results showed that there was good agreement between our proposed model and numerical simulation; moreover, our approach also gave promising calculation speed over numerical simulation. Some expected flow regimes were significantly distorted due to WIPS. The slope of type curves which characterize the linear or bi-linear flow regime is bigger than 0.5 or 0.25. The horizontal line which characterize radial flow regime is also bigger 0.5. The smaller the oil rate, the more severely flow regimes were distorted. Well rate mainly determines the distortion of MPI curves, while fracture length, well spacing, fracture spacing mainly determine when the distortion of the MPI curves occurs. The bigger the well rate, the more severely the MPI curves are distorted. While as the well spacing decreases, fracture length increases, fracture spacing increases, occurrence of MWPI become earlier. Stress sensitivity coefficient mainly affects the MPI at the formation pseudo-radial flow stage, almost has no influence on the occurrence of MWPI. This work gains some

Manual of selected physico-chemical analytical methods. IV